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

HRID 1714099
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HRID 1714099 반응식
[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]
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참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
78 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-574b3fa83f334e6895dd93809dad1299
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07795426B2

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