1-Methylpiperazine → HCID 178480926, 화합물

HRID 1852546노트

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HRID 1852546 반응식
[C:1]([O:5][C:6](=[O:19])[NH:7][C@H:8]1[CH2:13][CH2:12][C@H:11]([NH:14][C:15](=[O:18])[CH2:16]Cl)[CH2:10][CH2:9]1)([CH3:4])([CH3:3])[CH3:2].[CH3:20][N:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1>C(Cl)Cl>[C:1]([O:5][C:6](=[O:19])[NH:7][C@H:8]1[CH2:13][CH2:12][C@H:11]([NH:14][C:15](=[O:18])[CH2:16][N:24]2[CH2:25][CH2:26][N:21]([CH3:20])[CH2:22][CH2:23]2)[CH2:10][CH2:9]1)([CH3:4])([CH3:3])[CH3:2]

참가 물질

4

반응물 2

HCID 531671-MethylpiperazineHCID 178454048HCID 178454048, 화합물

생성물 1

HCID 178480926HCID 178480926, 화합물수율 59.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

A solution of trans-[4-(2-chloro-acetylamino)-cyclohexyl]-carbamic acid tert-butyl ester (330 mg, 1.14 mmol) in DCM (12 mL) was added to a solution of methylpiperazine (0.1 mL, 0.95 mmol) in DCM (1 mL) at RT. The resulting mixture was allowed to stir overnight, then diluted with DCM, and washed with a saturated aqueous solution of NaHCO3. The aqueous phase was extracted with DCM and then EtOAc. The combined organic phases were dried over Na2SO4, filtered and concentrated under reduced pressure to yield 199 mg of trans-{4-[2-(4-methyl-piperazin-1-yl)-acetylamino]-cyclohexyl}-carbamic acid tert-butyl ester without further purification.

후처리

  1. washwashed with a saturated aqueous solution of NaHCO3
  2. extractionThe aqueous phase was extracted with DCM
  3. dry with materialThe combined organic phases were dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-8c8b6446cf8949349a41122fc7bf6dca
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08962622B2

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