Hydrochloric Acid → (S)-8-chloro-1-(5-diethylaminomethyl-1,2,4-oxadiazol-3-yl)-11,12,13,13a-tetrahydro-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepin-9-one hydrochloride

HRID 1378203ノート

反応式

HRID 1378203 の反応式
[Cl:1][C:2]1[C:7]2[C:8](=[O:30])[N:9]3[CH2:29][CH2:28][CH2:27][C@H:10]3[C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]3[N:20]=[C:19]([CH2:21][N:22]([CH2:25][CH3:26])[CH2:23][CH3:24])[O:18][N:17]=3)[C:6]=2[CH:5]=[CH:4][CH:3]=1.Cl>C(O)C>[ClH:1].[Cl:1][C:2]1[C:7]2[C:8](=[O:30])[N:9]3[CH2:29][CH2:28][CH2:27][C@H:10]3[C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]3[N:20]=[C:19]([CH2:21][N:22]([CH2:25][CH3:26])[CH2:23][CH3:24])[O:18][N:17]=3)[C:6]=2[CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 22876632(S)-8-chloro-1-(5-diethylaminomethyl-1,2,4-oxadiazol-3-yl)-11,12,13,13a-tetrahydro-9H-imidazo-[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepin-9-one

生成物 1

HCID 70076595(S)-8-chloro-1-(5-diethylaminomethyl-1,2,4-oxadiazol-3-yl)-11,12,13,13a-tetrahydro-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepin-9-one hydrochloride収率 154.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

0.84 g (1.96 mmol) of (S)-8-chloro-1-(5-diethylaminomethyl-1,2,4-oxadiazol-3-yl)-11,12,13,13a-tetrahydro-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepin-9-one in 10 ml of ethanol was treated with 0.41 ml (1.96 mmol) of 4.78N ethanolic hydrochloric acid. After stirring at room temperature for 10 minutes the solution obtained was completely freed from the solvents. The residue was recrystallized from ethanol/ether. There was obtained 0.70 g (77%) of (S)-8-chloro-1-(5-diethylaminomethyl-1,2,4-oxadiazol-3-yl)-11,12,13,13a-tetrahydro-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepin-9-one hydrochloride (1:1) as white crystals; m.p. 205°-207° and [α]D20 =+25.2° (MeOH, c=1%).

後処理

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

出典と根拠

ORDレコード
ord-fa460c41c0514649bd623c2a60fbb764
出典データセット
uspto-grants-1997_09
特許番号
US05665718

反応ノート

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