Sodium borohydride → 5-hydroxymethyl-2-methyl-2H-1,2,3-triazole-4-carboxylic acid methyl ester
반응식
[CH3:1][O:2][C:3]([C:5]1[C:9]([CH:10]=[O:11])=[N:8][N:7]([CH3:12])[N:6]=1)=[O:4].[BH4-].[Na+]>CO>[CH3:1][O:2][C:3]([C:5]1[C:9]([CH2:10][OH:11])=[N:8][N:7]([CH3:12])[N:6]=1)=[O:4]참가 물질
4
실험 절차
2.6 g (13.3 mmol) of 5-formyl-2-methyl-2H-1,2,3-triazole-4-carboxylic acid methyl ester (see Example 2a) in methanol (100 ml) was treated with NaBH4 (601 mg) under stirring for 1 hour at ambient temperature. The reaction mixture was quenched with saturated aqueous ammonium chloride solution, extracted with ethyl acetate, dried with Na2SO4 and evaporated to give the crude as an oil. Purification on silica gel in ethyl acetate:hexane (2:1) yielded 1.85 g (81%) of the crystalline product, m.p. 112-113° C.
후처리
- customThe reaction mixture was quenched with saturated aqueous ammonium chloride solution
- extractionextracted with ethyl acetate
- dry with materialdried with Na2SO4
- customevaporated
- customto give the crude as an oil
- customPurification on silica gel in ethyl acetate:hexane (2:1)
출처 및 근거
- ORD 기록
- ord-90cd0e66b2174d1c9423d18c20cb532c
- 출처 데이터셋
- uspto-grants-2011_06
- 특허 번호
- US07956194B2
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