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Sodium borohydride → HCID 20344139, 화합물

HRID 2049663
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HRID 2049663 반응식
[BH4-].[Na+].Cl.[CH3:4][O:5][C:6]1[CH:7]=[C:8]([C:12](=[O:19])[CH2:13][CH:14]2[CH2:18][CH2:17][CH2:16][NH:15]2)[CH:9]=[CH:10][CH:11]=1>CO.O>[CH3:4][O:5][C:6]1[CH:7]=[C:8]([CH:12]([OH:19])[CH2:13][CH:14]2[CH2:18][CH2:17][CH2:16][NH:15]2)[CH:9]=[CH:10][CH:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 4311764Sodium borohydrideHCID 20344162HCID 20344162, 화합물

생성물 1

HCID 20344139HCID 20344139, 화합물수율 80%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

4.8 g of sodium borohydride are added portionwise with stirring to a solution of 6.5 g of 1-(3-methoxyphenyl)-2-(2-pyrrolidinyl)-ethanone hydrochloride in 25 ml of methanol and 5 ml of water. After 1 hour the bulk of the methanol is distilled off under a vacuum. The residue is taken up with 20 ml of water and 10 ml of 6 N sodium hydroxide solution. The mixture is extracted 5 times with, in each case, 20 ml of diethylether. The organic phases are collected, dried over sodium sulphate and concentrated to an oil which is distilled. 4.5 g of the title compound are obtained as mixture of diastereoisomers of b.p. 136° at 0.005 mm Hg.

후처리

  1. distillationAfter 1 hour the bulk of the methanol is distilled off under a vacuum
  2. extractionThe mixture is extracted 5 times with, in each case, 20 ml of diethylether
  3. customThe organic phases are collected
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated to an oil which
  6. distillationis distilled

출처 및 근거

ORD 기록
ord-75e3fda0aa234e69a856795cda88d449
출처 데이터셋
uspto-grants-1980_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04198424

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