Hydrochloric Acid → 9-(3-Dimethylamino-2-methylpropyl)-4,9-dihydro-4-methyl-10H-thieno[3,4-b][1,5]benzodiazepin-10-one, hydrochloride

HRID 436135ノート

反応式

HRID 436135 の反応式
[H-].[Na+].Cl.[CH3:4][N:5]([CH3:11])[CH2:6][CH:7]([CH3:10])[CH2:8][Cl:9].[CH3:12][N:13]1[C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=2[NH:17][C:16](=[O:24])[C:15]2=[CH:25][S:26][CH:27]=[C:14]12.Cl>CCOCC.CN(C)C=O>[ClH:9].[CH3:4][N:5]([CH3:11])[CH2:6][CH:7]([CH3:10])[CH2:8][N:17]1[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=2[N:13]([CH3:12])[C:14]2=[CH:27][S:26][CH:25]=[C:15]2[C:16]1=[O:24]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 24758Sodium hydrideHCID 30838413-Chloro-2-methylpropyl(dimethyl)ammonium chlorideHCID 12521642HCID 12521642、化合物

生成物 1

HCID 1317101519-(3-Dimethylamino-2-methylpropyl)-4,9-dihydro-4-methyl-10H-thieno[3,4-b][1,5]benzodiazepin-10-one, hydrochloride

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 0.47 g. of 55% sodium hydride-mineral oil dispersion and 0.91 g. of 3-dimethylamino-2-methylpropylchloride hydrochloride in 35 ml. of dry dimethylformamide is stirred at room temperature for 0.5 hours. To the mixture is added 0.6 g. of 4,9-dihydro-4-methyl-10H-thieno[3,4-b][1,5]-benzodiazepin-10-one and stirring is continued for 18 hours. The reaction mixture is cooled, quenched with water and extracted with chloroform. The dried chloroform extracts are concentrated to an oil, which is chromatographed on silica gel preparative thin layer chromatographic (tlc) plates with 10:1 benzene:methanol to give an oil. An ethanolic solution of the oil is treated with anhydrous hydrogen chloride and diluted with ether to give a white solid, m.p. 231°-233° C. (dec.).

後処理

  1. additionA mixture of 0.47 g
  2. additionTo the mixture is added 0.6 g
  3. temperatureThe reaction mixture is cooled
  4. customquenched with water
  5. extractionextracted with chloroform
  6. concentrationThe dried chloroform extracts are concentrated to an oil, which
  7. customis chromatographed on silica gel preparative thin layer chromatographic (tlc) plates with 10:1 benzene
  8. custommethanol to give an oil
  9. customto give a white solid, m.p. 231°-233° C. (dec.)

出典と根拠

ORDレコード
ord-fba65642a3c44c77a2a1b653bd2ba640
出典データセット
uspto-grants-1977_02
特許番号
US04007272

反応ノート

読み込み中…