Lauryl betaine synthesis
- Product Name:Lauryl betaine
- CAS Number:683-10-3
- Molecular formula:C16H33NO2
- Molecular Weight:271.45
Yield:683-10-3 99%
Reaction Conditions:
with Novovzym 435 in n-heptane at 65; for 5 h;Dean-Stark;Green chemistry;
Steps:
1 Comparative Example 1 Preparation of Lauryl Ν,Ν-Dimethylglycinate
Comparative Example 1 Preparation of Lauryl Ν,Ν-Dimethylglycinate [0170] Methyl 2-dimethylaminoacetate (189 g; 1 .61 mol; 1 .5 equiv), lauryl alcohol (200 g; 1 .07 mol), and Novovzym 435 (20 g) were combined in a 1 L 3-neck flask equipped with a Dean-Stark trap. 80 ml_ of heptane was added. The mixture was heated in a 65°C bath, and the pressure was reduced until a good overhead flow of the heptane/methanol azeotrope was obtained (ca. 110 mm Hg). After 5h, 99.1 % conversion to product was observed by NMR analysis. [0171] The reaction mixture was filtered to remove enzyme, the enzyme was washed with heptane, and the combined filtrate was concentrated to afford 289 g of lauryl N,N-dimethylaminoglycinate (99% yield). [0172] 1 H NMR (500 MHz, CDCI3) δ 4.13 (t, 2H); 3.16 (s, 2H); 2.35 (s, 6H); 1 .64 (m, 2H); 1.26 (s, 18H); 0.88 (t, 3H). [0173] HPLC (150 x 4.6 mm Zorbax SB-C8 column, 75:25 (v:v) methanol:water (containing 0.1 % trifluoroacetic acid) for 10 min, gradient to 100% methanol over 1 min, held at 100% methanol for 9 min, ELSD detection): tR 5.2 min.
References:
WO2017/48528,2017,A1 Location in patent:Paragraph 0170-0173
112-18-5
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683-10-3
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