Hydrochloric Acid → HCID 57551752、化合物

HRID 907266

反応式

HRID 907266 の反応式
[CH:1]1([NH:4][C:5](=[O:24])[C:6]2[CH:11]=[CH:10][C:9]([CH3:12])=[C:8]([C:13]3[CH:14]=[C:15]4[C:20](=[CH:21][CH:22]=3)[C:19](=[O:23])[NH:18][CH:17]=[CH:16]4)[CH:7]=2)[CH2:3][CH2:2]1.[H-].[Na+].C([O:30][C:31]1[CH:36]=[CH:35][C:34]([CH2:37]Cl)=[CH:33][CH:32]=1)(=O)C.[OH-].[Na+].Cl>CN(C=O)C>[CH:1]1([NH:4][C:5](=[O:24])[C:6]2[CH:11]=[CH:10][C:9]([CH3:12])=[C:8]([C:13]3[CH:14]=[C:15]4[C:20](=[CH:21][CH:22]=3)[C:19](=[O:23])[N:18]([CH2:37][C:34]3[CH:35]=[CH:36][C:31]([OH:30])=[CH:32][CH:33]=3)[CH:17]=[CH:16]4)[CH:7]=2)[CH2:2][CH2:3]1

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 24758Sodium hydride2 回HCID 1483124-(Chloromethyl)phenyl acetateHCID 25020457N-Cyclopropyl-4-methyl-3-(1-oxo-1,2-dihydro-isoquinolin-6-yl)-benzamide

生成物 1

HCID 57551752HCID 57551752、化合物収率 81.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of the product of Example 11 (460 mg) in DMF (10 mL) was added 60% sodium hydride (38 mg) and the reaction stirred at room temperature for 30 minutes before the addition of 4-(chloromethyl)phenyl acetate (280 mg). The reaction mixture was then stirred at room temperature for 17 hrs. Additional 60% sodium hydride (38 mg) was added and the reaction was stirred for a further 2 hours. NaOH (5N, 2 mL) was added and the reaction was stirred at room temperature for 90 minutes. The reaction mixture was acidified with HCl (2N) and extracted into ethyl acetate. The organics were washed with water and brine, dried over magnesium sulphate and evaporated to yield the sub-titled compound (500 mg).

後処理

  1. stirringthe reaction was stirred for a further 2 hours
  2. stirringthe reaction was stirred at room temperature for 90 minutes
  3. extractionextracted into ethyl acetate
  4. washThe organics were washed with water and brine
  5. dry with materialdried over magnesium sulphate
  6. customevaporated

出典と根拠

ORDレコード
ord-ab50e612b55a46608ff4714e6bba7b26
出典データセット
uspto-grants-2011_09
特許番号
US08012979B2

関連ノート

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