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Diethyl Ether → 7-[1-(Pyridin-4-yl)piperidin-4-ylmethoxy]-1,2,3,4-tetrahydroisoquinoline-2-carboxamidine dihydrochloride

HRID 412514
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HRID 412514 반응식
[N:1]1[CH:6]=[CH:5][C:4]([N:7]2[CH2:12][CH2:11][CH:10]([CH2:13][O:14][C:15]3[CH:24]=[C:23]4[C:18]([CH2:19][CH2:20][NH:21][CH2:22]4)=[CH:17][CH:16]=3)[CH2:9][CH2:8]2)=[CH:3][CH:2]=1.C(N(C(C)C)CC)(C)C.[ClH:34].[N:35]1([C:40](N)=[NH:41])C=CC=N1.C(OCC)C>CN(C)C=O>[ClH:34].[ClH:34].[N:1]1[CH:6]=[CH:5][C:4]([N:7]2[CH2:8][CH2:9][CH:10]([CH2:13][O:14][C:15]3[CH:24]=[C:23]4[C:18]([CH2:19][CH2:20][N:21]([C:40]([NH2:41])=[NH:35])[CH2:22]4)=[CH:17][CH:16]=3)[CH2:11][CH2:12]2)=[CH:3][CH:2]=1
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참가 물질

6

반응물 4

HCID 3283Diethyl EtherHCID 81531DiisopropylethylamineHCID 2734672Pyrazole-1-carboxamidine monohydrochlorideHCID 113247627-[1-(Pyridin-4-yl)piperidin-4-ylmethoxy]-1,2,3,4-tetrahydroisoquinoline

생성물 1

HCID 114419847-[1-(Pyridin-4-yl)piperidin-4-ylmethoxy]-1,2,3,4-tetrahydroisoquinoline-2-carboxamidine dihydrochloride수율 127.9%

시약·촉매·용매

1
HCID 6228Dimethylformamide용매

실험 절차

To a solution of 7-[1-(pyridin-4-yl)piperidin-4-ylmethoxy]-1,2,3,4-tetrahydroisoquinoline (50 mg) in dimethylformamide (0.5 ml) were added diisopropylethylamine (0.027 ml) and 1H-pyrazole-1-carboxamidine hydrochloride (23 mg), and the mixture was stirred at room temperature for 12 hours. After completion of the reaction, diethyl ether was added and insoluble material was collected by filtration. The obtained solid was washed with diethyl ether. A part (45 mg) of the obtained solid was treated with hydrogen chloride-methanol and dried under reduced pressure to give the title compound (44 mg).

후처리

  1. additionwas added
  2. filtrationinsoluble material was collected by filtration
  3. washThe obtained solid was washed with diethyl ether
  4. additionA part (45 mg) of the obtained solid was treated with hydrogen chloride-methanol
  5. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-f77bcf09cffb48e9b166fa6f843ca56a
출처 데이터셋
uspto-grants-2003_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06562828B1

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