Sodium borohydride → HCID 49760120、化合物

HRID 713183ノート

反応式

HRID 713183 の反応式
[F:1][C:2]1[CH:22]=[C:21]([F:23])[CH:20]=[CH:19][C:3]=1[C:4]([CH:6]1[CH2:11][CH2:10][N:9]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:8][CH2:7]1)=[O:5].[BH4-].[Na+]>CO>[F:1][C:2]1[CH:22]=[C:21]([F:23])[CH:20]=[CH:19][C:3]=1[CH:4]([OH:5])[CH:6]1[CH2:11][CH2:10][N:9]([C:12]([O:14][C:15]([CH3:17])([CH3:16])[CH3:18])=[O:13])[CH2:8][CH2:7]1

参加物

4

反応物 2

HCID 4311764Sodium borohydrideHCID 49760095tert-Butyl 4-(2,4-difluorobenzoyl)piperidine-1-carboxylate

生成物 1

HCID 49760120HCID 49760120、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a 0° C. solution of tert-butyl 4-(2,4-difluorobenzoyl)piperidine-1-carboxylate (1.28 g, 3.93 mmol) in MeOH (15.7 mL) was added NaBH4 (0.372 g, 9.84 mmol). The ice bath was removed and the reaction mixture stirred for 2 h at room temperature then was quenched with saturated aqueous NH4Cl. The organic layer was extracted with EtOAc, washed with H2O and dried over MgSO4. The solvent was removed under reduced pressure gave tert-butyl 4-((2,4-difluorophenyl)(hydroxy)methyl)piperidine-1-carboxylate as a white hygroscopic solid.

後処理

  1. customThe ice bath was removed
  2. customthen was quenched with saturated aqueous NH4Cl
  3. extractionThe organic layer was extracted with EtOAc
  4. washwashed with H2O
  5. dry with materialdried over MgSO4
  6. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-982a4f4aff0b4771b17ddf158a892c31
出典データセット
uspto-grants-2015_11
特許番号
US09181249B2

反応ノート

読み込み中…