Hydrochloric Acid → 3-(4-diallylaminomethyl-thiazol-2-yl)-8-fluoro-5-methyl-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepin-6-one hydrochloride

HRID 1737375ノート

反応式

HRID 1737375 の反応式
[CH2:1]([N:4]([CH2:8][C:9]1[N:10]=[C:11]([C:14]2[N:15]=[CH:16][N:17]3[C:23]4[CH:24]=[CH:25][C:26]([F:28])=[CH:27][C:22]=4[C:21](=[O:29])[N:20]([CH3:30])[CH2:19][C:18]=23)[S:12][CH:13]=1)[CH2:5][CH:6]=[CH2:7])[CH:2]=[CH2:3].[ClH:31]>C(O)C>[ClH:31].[CH2:1]([N:4]([CH2:8][C:9]1[N:10]=[C:11]([C:14]2[N:15]=[CH:16][N:17]3[C:23]4[CH:24]=[CH:25][C:26]([F:28])=[CH:27][C:22]=4[C:21](=[O:29])[N:20]([CH3:30])[CH2:19][C:18]=23)[S:12][CH:13]=1)[CH2:5][CH:6]=[CH2:7])[CH:2]=[CH2:3]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 218422383-(4-diallylaminomethyl-thiazol-2-yl)-8-fluoro-5-methyl-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepin-6-one

生成物 1

HCID 218422373-(4-diallylaminomethyl-thiazol-2-yl)-8-fluoro-5-methyl-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepin-6-one hydrochloride収率 80%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

0.90 g (0.00212 mol) of 3-(4-diallylaminomethyl-thiazol-2-yl)-8-fluoro-5-methyl-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepin-6-one in 40 ml of ethanol was treated with 0.45 ml (0.00215 mol) of 4.78N ethanolic hydrochloric acid. After stirring at room temperature for 15 minutes the solution obtained was completely freed from the solvents. The residue was recrystallized from ethanol/ether. There was obtained 0.78 g (80%) of 3-(4-diallylaminomethyl-thiazol-2-yl)-8-fluoro-5-methyl-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepin-6-one hydrochloride (1:1) as white crystals; m.p. 152-155°.

後処理

  1. customobtained
  2. customThe residue was recrystallized from ethanol/ether

出典と根拠

ORDレコード
ord-604e3bba0a7f4438b29b181c1ebcb06b
出典データセット
uspto-grants-1999_10
特許番号
US05962450

反応ノート

読み込み中…