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 2280214ノート

反応式

HRID 2280214 の反応式
[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]

参加物

4

反応物 2

HCID 21866389Hydrogen chloride-ethyl acetate2 回HCID 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

生成物 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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-85cc2ff5c6614448a680fb910f103bc2
出典データセット
uspto-grants-2015_09
特許番号
US09138434B2

反応ノート

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