Methanol → HCID 59625678、化合物

HRID 1023037

反応式

HRID 1023037 の反応式
C([N:14]1[CH2:17][CH:16]([N:18]2[CH2:23][CH2:22][N:21]([C:24](=[O:29])[C:25]([F:28])([F:27])[F:26])[CH2:20][CH2:19]2)[CH2:15]1)(C1C=CC=CC=1)C1C=CC=CC=1.ClC(OC(Cl)C)=O.CO.CCOCC>C(Cl)Cl>[NH:14]1[CH2:15][CH:16]([N:18]2[CH2:19][CH2:20][N:21]([C:24](=[O:29])[C:25]([F:26])([F:27])[F:28])[CH2:22][CH2:23]2)[CH2:17]1

参加物

6

反応物 4

HCID 887MethanolHCID 3283Diethyl EtherHCID 5213051-Chloroethyl chloroformateHCID 596259751-[4-(1-Benzhydryl-azetidin-3-yl)-piperazin-1-yl]-2,2,2-trifluoro-ethanone

生成物 1

HCID 59625678HCID 59625678、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

To a solution of compound 1f (2.11 g, 5.23 mmol) in CH2Cl2 (60 mL) was added 1-chloroethyl chloroformate (2.0 mL, 18.35 mmol) at 0° C. under N2. The mixture was stirred at 0° C. for 90 min and then MeOH (4 mL) was added. The mixture was refluxed for 1 h. Upon cooling, Et2O (50 mL) was added to the mixture. The resulting solid was collected by filtration and dried. The crude compound 1g was used in the next reaction without further purification. MS m/z (M+H+) 238.1.

後処理

  1. temperatureThe mixture was refluxed for 1 h
  2. temperatureUpon cooling
  3. filtrationThe resulting solid was collected by filtration
  4. customdried
  5. customThe crude compound 1g was used in the next reaction without further purification

出典と根拠

ORDレコード
ord-23d6608803644724bf564ba60ef01701
出典データセット
uspto-grants-2014_05
特許番号
US08722658B2

関連ノート

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