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Fumaric Acid → 10-[(2RS)-1-diethylamino-2-propyl]-N-(2-methylpropyl)-2-phenothiazinecarboxamide fumarate

HRID 728716
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반응식

HRID 728716 반응식
[C:1]([OH:8])(=[O:7])/[CH:2]=[CH:3]/[C:4]([OH:6])=[O:5].[CH2:9]([N:11]([CH2:36][CH3:37])[CH2:12][CH:13]([N:15]1[C:28]2[CH:27]=[C:26]([C:29]([NH:31][CH2:32][CH:33]([CH3:35])[CH3:34])=[O:30])[CH:25]=[CH:24][C:23]=2[S:22][C:21]2[C:16]1=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH3:14])[CH3:10]>CC(O)C>[C:1]([OH:8])(=[O:7])/[CH:2]=[CH:3]/[C:4]([OH:6])=[O:5].[CH2:36]([N:11]([CH2:9][CH3:10])[CH2:12][CH:13]([N:15]1[C:28]2[CH:27]=[C:26]([C:29]([NH:31][CH2:32][CH:33]([CH3:35])[CH3:34])=[O:30])[CH:25]=[CH:24][C:23]=2[S:22][C:21]2[C:16]1=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH3:14])[CH3:37]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 444972Fumaric AcidHCID 1453657110-[(2RS)-1-diethylamino-2-propyl]-N-(2-methylpropyl)-2-phenothiazinecarboxamide

생성물 1

HCID 1453657210-[(2RS)-1-diethylamino-2-propyl]-N-(2-methylpropyl)-2-phenothiazinecarboxamide fumarate수율 80.5%

시약·촉매·용매 1

HCID 3776Isopropanol용매2회

실험 절차

Fumaric acid (0.18 g) dissolved in 2-propanol (7.5 cc) under reflux is added to a solution of 10-[(2RS)-1-diethylamino-2-propyl]-N-(2-methylpropyl)-2-phenothiazinecarboxamide (0.62 g) in boiling 2-propanol (7.5 cc). The mixture is concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C. and the residue is stirred in isopropyl ether (50 cc). The solid is separated by filtration on sintered glass, washed with isopropyl ether (10 cc) and dried under reduced pressure (5 mm Hg; 0.7 kPa) to give 10-[(2RS)-1-diethylamino-2-propyl]-N-(2-methylpropyl)-2-phenothiazinecarboxamide fumarate (0.64 g), m.p. 110° C.

후처리

  1. temperatureunder reflux
  2. concentrationThe mixture is concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C.
  3. customThe solid is separated by filtration on sintered glass
  4. washwashed with isopropyl ether (10 cc)
  5. customdried under reduced pressure (5 mm Hg; 0.7 kPa)

출처 및 근거

ORD 기록
ord-de8258936fa747c49401092510a7fdb3
출처 데이터셋
uspto-grants-1991_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05049669

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