Sodium borohydride → 2-(4-Chlorophenyl)cyclobutanamine

HRID 1482439노트

반응식

HRID 1482439 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[CH2:11][CH2:10][C:9]2=[N:12]O)=[CH:4][CH:3]=1.[BH4-].[Na+]>CO>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH:8]2[CH2:11][CH2:10][CH:9]2[NH2:12])=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 4311764Sodium borohydrideHCID 1317367062-(4-Chlorophenyl)cyclobutanone oxime

생성물 1

HCID 810131342-(4-Chlorophenyl)cyclobutanamine수율 66.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 2-(4-chlorophenyl)cyclobutanone oxime (200 mg, 1 mmol) in methanol (5 ml) was added MoO3 (205 mg, 1.4 eq.) and sodium borohydride (394 mg, 10 eq) at 0° C. After stirring at rt for 2 h the solvent was evaporated. A mixture of H2O and CH2Cl2 was added. Organic phase was separated, washed with brine, dried and concentrated in vacuo. 120 mg of product-amine was isolated as a mixture of cis and trans isomers 2:1. The crude product without purification was used for the next reaction.

후처리

  1. customwas evaporated
  2. additionA mixture of H2O and CH2Cl2
  3. additionwas added
  4. customOrganic phase was separated
  5. washwashed with brine
  6. customdried
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-f804baaaeea3454cb98a328cec5f7536
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09414589B2

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