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Water → (4-Isopropyl-piperazin-1-yl)-(4-morpholin-4-ylmethyl-phenyl)-methanone, dihydrochloride monohydrate

HRID 560978
ノート
印刷プレビュー

反応式

HRID 560978 の反応式
[ClH:1].Cl.[CH:3]([N:6]1[CH2:11][CH2:10][N:9]([C:12]([C:14]2[CH:19]=[CH:18][C:17]([CH2:20][N:21]3[CH2:26][CH2:25][O:24][CH2:23][CH2:22]3)=[CH:16][CH:15]=2)=[O:13])[CH2:8][CH2:7]1)([CH3:5])[CH3:4].O.CC(OC)(C)C>CCO>[OH2:13].[ClH:1].[ClH:1].[CH:3]([N:6]1[CH2:11][CH2:10][N:9]([C:12]([C:14]2[CH:15]=[CH:16][C:17]([CH2:20][N:21]3[CH2:22][CH2:23][O:24][CH2:25][CH2:26]3)=[CH:18][CH:19]=2)=[O:13])[CH2:8][CH2:7]1)([CH3:5])[CH3:4]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 15413tert-Butyl methyl etherHCID 67038973(4-Isopropyl-piperazin-1-yl)-(4-morpholin-4-ylmethyl-phenyl)-methanone, dihydrochloride

生成物 1

HCID 131728157(4-Isopropyl-piperazin-1-yl)-(4-morpholin-4-ylmethyl-phenyl)-methanone, dihydrochloride monohydrate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
78 °C

実験手順

A suspension of crude (4-isopropyl-piperazin-1-yl)-(4-morpholin-4-ylmethyl-phenyl)-methanone, dihydrochloride (2.1 g, 5.2 mmol) in absolute EtOH (30 mL) was heated to 78° C. and H2O (2.2 mL) was added. The resulting solution was cooled to room temperature and MTBE (5 mL) was added. The resulting suspension was cooled to 0° C. and filtered. The filter cake was washed with MeOH (15 mL). The solids were dried in a vacuum oven at 105° C. for 20 h to yield the title compound as a white solid.

後処理

  1. temperatureThe resulting solution was cooled to room temperature
  2. temperatureThe resulting suspension was cooled to 0° C.
  3. filtrationfiltered
  4. washThe filter cake was washed with MeOH (15 mL)
  5. customThe solids were dried in a vacuum oven at 105° C. for 20 h

出典と根拠

ORDレコード
ord-4ca859f34b66435ca8dc2d0e99e97e14
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08063206B2

反応ノート

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