1-Methylpiperazine → HCID 178480926、化合物

HRID 1852546ノート

反応式

HRID 1852546 の反応式
[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]

参加物

4

反応物 2

HCID 531671-MethylpiperazineHCID 178454048HCID 178454048、化合物

生成物 1

HCID 178480926HCID 178480926、化合物収率 59.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8c8b6446cf8949349a41122fc7bf6dca
出典データセット
uspto-grants-2015_02
特許番号
US08962622B2

反応ノート

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