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 1378203노트

반응식

HRID 1378203 반응식
[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

참가 물질

4

반응물 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

생성물 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 hydrochloride수율 154.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-fa460c41c0514649bd623c2a60fbb764
출처 데이터셋
uspto-grants-1997_09
특허 번호
US05665718

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