Sodium borohydride → HCID 67115789、化合物

HRID 1258811ノート

反応式

HRID 1258811 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([Cl:25])=[C:6]([CH:24]=1)[CH2:7][C:8]1[CH:9]=[CH:10][C:11]2[O:16][CH2:15][CH2:14][N:13](C(=O)C(F)(F)F)[C:12]=2[CH:23]=1.[BH4-].[Na+]>C(O)C>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([Cl:25])=[C:6]([CH:24]=1)[CH2:7][C:8]1[CH:9]=[CH:10][C:11]2[O:16][CH2:15][CH2:14][NH:13][C:12]=2[CH:23]=1

参加物

4

反応物 2

HCID 4311764Sodium borohydrideHCID 583408561-[6-(5-Bromo-2-chloro-benzyl)-2,3-dihydro-benzo[1,4]oxazin-4-yl]-2,2,2-trifluoro-ethanone

生成物 1

HCID 67115789HCID 67115789、化合物収率 91%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a stirred solution of 1-[6-(5-bromo-2-chloro-benzyl)-2,3-dihydro-benzo[1,4]oxazin-4-yl]-2,2,2-trifluoro-ethanone (8.6 g, 19.8 mmol) in ethanol (40 mL) was added NaBH4 portion wise and the reaction mixture was stirred overnight. The excess of NaBH4 was quenched by adding aq. HCl. Ethanol was evaporated and the residue was partitioned between dichloromethane and water. Organic layer was washed with brine, water, dried over sodium sulfate followed by evaporation of solvent furnished 6-(5-bromo-2-chloro-benzyl)-3,4-dihydro-2H-benzo[1,4]oxazine (6.1 g).

後処理

  1. customThe excess of NaBH4 was quenched
  2. additionby adding aq. HCl
  3. customEthanol was evaporated
  4. customthe residue was partitioned between dichloromethane and water
  5. washOrganic layer was washed with brine, water
  6. dry with materialdried over sodium sulfate
  7. customfollowed by evaporation of solvent

出典と根拠

ORDレコード
ord-f783194df348432c99ac5cedf2dd227a
出典データセット
uspto-grants-2013_06
特許番号
US08466114B2

反応ノート

読み込み中…