Lithium borohydride → 2-(2,2,2-Trifluoro-ethoxy)-4-hydroxymethyl-benzonitrile
반응식
C[O:2][C:3](=O)[C:4]1[CH:9]=[CH:8][C:7]([C:10]#[N:11])=[C:6]([O:12][CH2:13][C:14]([F:17])([F:16])[F:15])[CH:5]=1.[Li+].[BH4-]>C1COCC1>[F:15][C:14]([F:16])([F:17])[CH2:13][O:12][C:6]1[CH:5]=[C:4]([CH2:3][OH:2])[CH:9]=[CH:8][C:7]=1[C:10]#[N:11]참가 물질
4
반응 조건
- 온도
- 70 °C
실험 절차
4-Cyano-3-(2,2,2-trifluoro-ethoxy)-benzoic acid methyl ester from step 1 (1.6 g, 6.2 mmol ) was dissolved in THF (62 ml). LiBH4 in THF (2M, 6.2 ml, 12.4 mmol) was added. The reaction mixture was heated to 70° C. for 3 hours. The reaction was quenched carefully with 3N HCl and then extracted with EtOAc (3×10 mL). The organic layers were combined, washed with brine, dried (MgSO4) filtered and concentrated to yield the desired product.
후처리
- customThe reaction was quenched carefully with 3N HCl
- extractionextracted with EtOAc (3×10 mL)
- washwashed with brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-4368df320f96498f90a6aa62ec1d9530
- 출처 데이터셋
- uspto-grants-1999_08
- 특허 번호
- US05939439
반응 노트
불러오는 중…