Hydrochloric Acid → 3-(3-(((7S)-3,4-dimethoxy-7-bicyclo(4.2.0)octa-1,3,5-trienyl)methylamino)propyl)-7,8-dimethoxy-2,5-dihydro-1H-3-benzazepin-4-one;hydrochloride

HRID 423131ノート

反応式

HRID 423131 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:8](=[CH:9][C:10]=1[O:11][CH3:12])[C@@H:7]([CH2:13][NH:14][CH2:15][CH2:16][CH2:17][N:18]1[C:24](=[O:25])[CH2:23][C:22]3[CH:26]=[C:27]([O:32][CH3:33])[C:28]([O:30][CH3:31])=[CH:29][C:21]=3[CH2:20][CH2:19]1)[CH2:6]2.[ClH:34]>C(#N)C.C(OCC)C>[ClH:34].[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:8](=[CH:9][C:10]=1[O:11][CH3:12])[C@@H:7]([CH2:13][NH:14][CH2:15][CH2:16][CH2:17][N:18]1[C:24](=[O:25])[CH2:23][C:22]3[CH:26]=[C:27]([O:32][CH3:33])[C:28]([O:30][CH3:31])=[CH:29][C:21]=3[CH2:20][CH2:19]1)[CH2:6]2

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 10389261N-Demethylivabradine

生成物 1

HCID 666726993-(3-(((7S)-3,4-dimethoxy-7-bicyclo(4.2.0)octa-1,3,5-trienyl)methylamino)propyl)-7,8-dimethoxy-2,5-dihydro-1H-3-benzazepin-4-one;hydrochloride収率 72.1%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6342Acetonitrile溶媒

実験手順

300 mg (0.65 mmol) of the amine obtained in Example 2, Step 2, are dissolved in 10 mL of acetonitrile. To the resulting solution there is added 0.65 mL (1.3 mmol, 2 equivalents) of 2M hydrochloric acid solution in diethyl ether. Stirring is carried out at 25° C. for 15 minutes, and then evaporation to dryness. The product is crystallised from 20 mL of acetone. The solid is filtered off and dried. 230 mg of white crystals are obtained.

後処理

  1. customevaporation to dryness
  2. customThe product is crystallised from 20 mL of acetone
  3. filtrationThe solid is filtered off
  4. customdried

出典と根拠

ORDレコード
ord-2d9610d533be42abacb334f404b541fb
出典データセット
uspto-grants-2012_01
特許番号
US08101747B2

反応ノート

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