2-(4-BROMOPHENYL)-2-(HYDROXYMETHYL)PROPANE-1,3-DIOL synthesis
- Product Name:2-(4-BROMOPHENYL)-2-(HYDROXYMETHYL)PROPANE-1,3-DIOL
- CAS Number:936494-74-5
- Molecular formula:C10H13BrO3
- Molecular Weight:261.11
1423702-61-7
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Yield:936494-74-5 85.14%
Reaction Conditions:
with lithium aluminium tetrahydride in tetrahydrofuran at 20 - 60; for 2.2 h;
Steps:
3.1.2 Step 2: Preparation of Intermediate 3-1b
At room temperature, to LiAlH4(7.51 g, 197.92 mmol) in THF (300 mL) was added dropwise to a solution of Intermediate 3-1a (30 g, 98.96 mmol) in THF (100 mL).The mixture was stirred at room temperature for 20 minutes, and then heated to 60°C and stirred for 2 hours.After cooling to room temperature, the reaction solution was quenched with ice water, and then added aq.HC1 (2N) to adjust the pH to 2-3, the mixture was extracted with n-butanol, the combined organic phase was concentrated, and the crude product was separated and purified with a silica gel column (DCM :MeOH=10:1, v/v) to obtain 3-1b (22g, 84.26mmol, 85.14% yield),
References:
CN112341439,2021,A Location in patent:Paragraph 0140-0142; 0145-0146
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