5-(4-CHLORO-BENZYL)-[1,3,4]THIADIAZOL-2-YLAMINE synthesis
- Product Name:5-(4-CHLORO-BENZYL)-[1,3,4]THIADIAZOL-2-YLAMINE
- CAS Number:39181-43-6
- Molecular formula:C9H8ClN3S
- Molecular Weight:225.7
39202-97-6
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39181-43-6
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Yield:39181-43-6 79%
Reaction Conditions:
Stage #1: 2-[(4-chlorophenyl)acetyl]hydrazinecarbothioamidewith phosphorus tribromide at 60; for 16 h;
Stage #2: with ammonia in water; pH=9;
Steps:
A mixture of the 2-[(4-chlorophenyl)acetyl]hydrazinecarbothioamide (Intermediate 64) (5g, 0.020 mol.) and PBr3 (30 ml_, 0.146 mol.) was heated at 600C for 16 hours. Then the reaction was poured into ice-water and the pH was adjusted to 9 with ammonia. After filtration of the suspension, the solid material was dried to give the title compound as a solid (3.6 g, 79%). LC/MS: m/z 226 (M+H) Rt: 3.55 min.
References:
WO2008/104524,2008,A1 Location in patent:Page/Page column 56-57
