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

HRID 524065ノート

反応式

HRID 524065 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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]+.

後処理

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

出典と根拠

ORDレコード
ord-f92e3d0fba914e01ab94fd4323a0bf90
出典データセット
uspto-grants-2016_05
特許番号
US09340514B2

反応ノート

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