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

HRID 412514
ノート
印刷プレビュー

反応式

HRID 412514 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒

1
HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-f77bcf09cffb48e9b166fa6f843ca56a
出典データセット
uspto-grants-2003_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06562828B1

反応ノート

読み込み中…

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