Dichloromethane → 9-Chloro-7-(2-chlorophenyl)-5H-pyrimido(5,4-d)(2)benzazepine

HRID 464512ノート

反応式

HRID 464512 の反応式
[C:1](O)(=O)C.[CH:5]([NH2:7])=[NH:6].C[O-].[Na+].[Cl:11][C:12]1[CH:34]=[CH:33][C:15]2[C:16](=O)[CH2:17][C:18](=CN(C)C)[N:19]=[C:20]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23]C=3Cl)[C:14]=2[CH:13]=1.[CH2:35]([Cl:37])Cl>CO.O>[Cl:11][C:12]1[CH:34]=[CH:33][C:15]2[C:16]3[N:7]=[CH:5][N:6]=[CH:1][C:17]=3[CH2:18][N:19]=[C:20]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][C:35]=3[Cl:37])[C:14]=2[CH:13]=1

参加物

7

反応物 4

HCID 6344DichloromethaneHCID 160693Formamidine acetateHCID 10942334Sodium MethoxideHCID 572766058-chloro-1-(2-chlorophenyl)-3,4-dihydro-[(dimethylamino)methylene]-5H-2-benzazepin-5-one

生成物 1

HCID 1317369-Chloro-7-(2-chlorophenyl)-5H-pyrimido(5,4-d)(2)benzazepine

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 962Water溶媒

実験手順

In five equal portions 21 g (200 mmole) of formamidine acetate and 32.5 ml (135 mmole) of a 4.12M methanol solution of sodium methoxide was added over 3 hr to a solution of 7.2 g (20 mmole) of 8-chloro-1-(2-chlorophenyl)-3,4-dihydro-[(dimethylamino)methylene]-5H-2-benzazepin-5-one in 270 ml of methanol and 270 ml of methylene chloride. The solution was diluted with water and extracted with methylene chloride. The methylene chloride solution was washed with water, dried over anhydrous sodium sulfate, and concentrated at reduced pressure to give an amber oil. Purification by column chromatography (100 g silica gel; eluent 1:1 methylene chloride and ethyl acetate) gave end product mp 122°-124° C. Recrystallization from ether gave pale yellow prisms, mp 122°-125° C.

後処理

  1. extractionextracted with methylene chloride
  2. washThe methylene chloride solution was washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated at reduced pressure
  5. customto give an amber oil
  6. customPurification by column chromatography (100 g silica gel; eluent 1:1 methylene chloride and ethyl acetate)

出典と根拠

ORDレコード
ord-d80e90c64b2c4282a1256f72e39bbb51
出典データセット
uspto-grants-1985_10
特許番号
US04547581

反応ノート

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