4-Amino-1-Boc-piperidine → 1,1-Dimethylethyl 4-({[(2-fluoro-6-iodo-4-methylphenyl)amino]-carbonyl}amino)-1-piperidinecarboxylate

HRID 447753노트

반응식

HRID 447753 반응식
[F:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]([I:9])[C:3]=1[N:10]=[C:11]=[O:12].[NH2:13][CH:14]1[CH2:19][CH2:18][N:17]([C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21])[CH2:16][CH2:15]1>ClCCl>[F:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]([I:9])[C:3]=1[NH:10][C:11]([NH:13][CH:14]1[CH2:15][CH2:16][N:17]([C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21])[CH2:18][CH2:19]1)=[O:12]

참가 물질

4

반응물 2

HCID 12682914-Amino-1-Boc-piperidineHCID 866189401-Fluoro-3-iodo-2-isocyanato-5-methylbenzene2회

생성물 1

HCID 596832811,1-Dimethylethyl 4-({[(2-fluoro-6-iodo-4-methylphenyl)amino]-carbonyl}amino)-1-piperidinecarboxylate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of the crude 1-fluoro-3-iodo-2-isocyanato-5-methylbenzene from description D2, 4-amino-1-N-Boc piperidine (200 mg, 1 mmol), and dichloromethane (3 ml) was stirred at room temperature for 1 h then directly purified by chromatography on silica gel eluting with 0 to 10% methanol in dichloromethane. Further purification by MDAP (mass-directed auto-purification) gave the title compound 300 mg.

후처리

  1. customthen directly purified by chromatography on silica gel eluting with 0 to 10% methanol in dichloromethane
  2. customFurther purification
  3. customby MDAP (mass-directed auto-purification)

출처 및 근거

ORD 기록
ord-787e6f1d9bf9421380ef7ecd92e08c6a
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08481566B2

반응 노트

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