Hydrogen chloride-ethyl acetate → 1-{[(4aR*,6R*,8aR*)-3-Cyano-8-methyl-2-(methylamino)-4H,4aH,5H,6H,7H,8H,8aH,9H-thieno[3,2-g]quinolin-6-yl]carbonyl}-3-[2-(dimethylamino)ethyl]-1-propylurea di hydrochloride salt

HRID 2280214노트

반응식

HRID 2280214 반응식
[C:1]([C:3]1[C:7]2[CH2:8][C@@H:9]3[C@@H:14]([CH2:15][C:6]=2[S:5][C:4]=1[N:31](C)[C:32](=O)OC(C)(C)C)[N:13]([CH3:16])[CH2:12][C@H:11]([C:17]([N:19]([C:23](=[O:30])[NH:24][CH2:25][CH2:26][N:27]([CH3:29])[CH3:28])[CH2:20][CH2:21][CH3:22])=[O:18])[CH2:10]3)#[N:2].C(OCC)(=O)C.[ClH:46]>C(OCC)(=O)C>[ClH:46].[ClH:46].[C:1]([C:3]1[C:7]2[CH2:8][C@@H:9]3[C@@H:14]([CH2:15][C:6]=2[S:5][C:4]=1[NH:31][CH3:32])[N:13]([CH3:16])[CH2:12][C@H:11]([C:17]([N:19]([CH2:20][CH2:21][CH3:22])[C:23]([NH:24][CH2:25][CH2:26][N:27]([CH3:28])[CH3:29])=[O:30])=[O:18])[CH2:10]3)#[N:2]

참가 물질

4

반응물 2

HCID 21866389Hydrogen chloride-ethyl acetate2회HCID 86731029tert-butyl N-[(4aR*,6R*,8aR*)-3-cyano-6-[({[2-(dimethylamino)ethyl]carbamoyl}(propyl)amino)carbonyl]-8-methyl-4H,4aH,5H,6H,7H,8H,8aH,9H-thieno[3,2-g]quinolin-2-yl]-N-methylcarbamate

생성물 1

HCID 867310301-{[(4aR*,6R*,8aR*)-3-Cyano-8-methyl-2-(methylamino)-4H,4aH,5H,6H,7H,8H,8aH,9H-thieno[3,2-g]quinolin-6-yl]carbonyl}-3-[2-(dimethylamino)ethyl]-1-propylurea di hydrochloride salt

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To a mixture of tert-butyl N-[(4aR*,6R*,8aR*)-3-cyano-6-[({[2-(dimethylamino)ethyl]carbamoyl}(propyl)amino)carbonyl]-8-methyl-4H,4aH,5H,6H,7H,8H,8aH,9H-thieno[3,2-g]quinolin-2-yl]-N-methylcarbamate (160 mg) and ethyl acetate (10 mL) was added a 4 mol/L hydrogen chloride-ethyl acetate solution (5 mL) while stirring at room temperature, and the mixture was stirred at the same temperature for 11 hours. To the reaction mixture was added a 4 mol/L hydrogen chloride-ethyl acetate solution (5 mL) while stirring at room temperature, and then stirred at the same temperature for 13 hours. The solid was collected by filtration to give the title compound (compound 3-1) (116 mg). The structure was illustrated in Table 11.

후처리

  1. stirringthe mixture was stirred at the same temperature for 11 hours
  2. stirringwhile stirring at room temperature
  3. stirringstirred at the same temperature for 13 hours
  4. filtrationThe solid was collected by filtration

출처 및 근거

ORD 기록
ord-85cc2ff5c6614448a680fb910f103bc2
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09138434B2

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