Hydrochloric Acid → HCID 178484004、化合物

HRID 245748ノート

反応式

HRID 245748 の反応式
C(O[C:9](=O)[N:10]([CH2:12][C@H:13]1[CH2:18][CH2:17][C@H:16]([C:19]2[N:23]3[CH:24]=[CH:25][N:26]=[C:27]([CH3:28])[C:22]3=[C:21]([Br:29])[N:20]=2)[CH2:15][CH2:14]1)C)C1C=CC=CC=1.Cl>>[Br:29][C:21]1[N:20]=[C:19]([C@H:16]2[CH2:17][CH2:18][C@H:13]([CH2:12][NH:10][CH3:9])[CH2:14][CH2:15]2)[N:23]2[CH:24]=[CH:25][N:26]=[C:27]([CH3:28])[C:22]=12

参加物

3

反応物 2

HCID 313Hydrochloric AcidHCID 178432909HCID 178432909、化合物

生成物 1

HCID 178484004HCID 178484004、化合物収率 90.2%

実験手順

The impure benzyl((trans)-4-(1-bromo-8-methylimidazo[1,5-a]pyrazin-3-yl)cyclohexyl)methyl(methyl)carbamate (0.299 mmol, 141 mg) in 37% hydrochloric acid (20.94 mmol, 1.745 ml) was stirred for 18 hours at room temperature and one hour at 40° C. The reaction mixture was concentrated in vacuo. The residue dissolved in water and washed with diethyl ether twice. The aqueous layer basified with 2 N aqueous sodium hydroxide and extracted with dichloromethane twice. The combined organic extracts were dried (Na2SO4) and concentrated in vacuo to give impure 1-((trans)-4-(1-bromo-8-methylimidazo[1,5-a]pyrazin-3-yl)cyclohexyl)-N-methylmethanamine (91 mg).

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. dissolutionThe residue dissolved in water
  3. washwashed with diethyl ether twice
  4. extractionextracted with dichloromethane twice
  5. dry with materialThe combined organic extracts were dried (Na2SO4)
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-1cbfc8152b784258ab37e538c23b5302
出典データセット
uspto-grants-2014_02
特許番号
US08658794B2

反応ノート

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