Aluminium lithium hydride → (6-Chloro-5-methyl-4-(methylamino)pyridin-3-yl)methanol

HRID 2274209노트

반응식

HRID 2274209 반응식
[Cl:1][C:2]1[C:12]([CH3:13])=[C:11]([NH:14][CH3:15])[C:5]([C:6](OCC)=[O:7])=[CH:4][N:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-]>O1CCCC1>[Cl:1][C:2]1[N:3]=[CH:4][C:5]([CH2:6][OH:7])=[C:11]([NH:14][CH3:15])[C:12]=1[CH3:13]

참가 물질

4

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 86713588Ethyl 6-chloro-5-methyl-4-(methylamino)nicotinate

생성물 1

HCID 86713589(6-Chloro-5-methyl-4-(methylamino)pyridin-3-yl)methanol수율 85.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of ethyl 6-chloro-5-methyl-4-(methylamino)nicotinate (2.0 g, 8.8 mmol) in tetrahydrofuran (60 mL) was added lithium aluminium hydride at 0° C., and the mixture was stirred at RT for 1.5 h. LCMS monitored the reaction was completed. The reaction was quenched by sodium sulfate decahydrate (1.5 g) and filtrated. The filtrate was concentrated to get the title compound (1.4 g, crude) as a white solid. MS (ES+) C8H11ClN2O requires: 186, 188. Found: 187, 189 [M+H]+.

후처리

  1. customThe reaction was quenched by sodium sulfate decahydrate (1.5 g)
  2. filtrationfiltrated
  3. concentrationThe filtrate was concentrated

출처 및 근거

ORD 기록
ord-fdc731ee568d49cd83aba581ac46219d
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09126951B2

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