Sodium borohydride → HCID 67115789, 화합물

HRID 72567노트

반응식

HRID 72567 반응식
[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

참가 물질

4

반응물 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

생성물 1

HCID 67115789HCID 67115789, 화합물수율 91%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-b047f4e6a36947998d827108c4b7083d
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08828951B2

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