Sodium hydride → HCID 58626094、化合物

HRID 1161696

反応式

HRID 1161696 の反応式
[CH3:1][C:2]([C:4]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[C:6]([Cl:12])[CH:5]=1)=[O:3].[H-].[Na+].C([O:17][C:18](=O)[C:19]1[CH:24]=[CH:23][CH:22]=[N:21][CH:20]=1)C>CN(C=O)C>[Cl:12][C:6]1[CH:5]=[C:4]([C:2](=[O:3])[CH2:1][C:18]([C:19]2[CH:20]=[N:21][CH:22]=[CH:23][CH:24]=2)=[O:17])[CH:9]=[CH:8][C:7]=1[O:10][CH3:11]

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 69188Ethyl NicotinateHCID 5208573'-Chloro-4'-methoxyacetophenone

生成物 1

HCID 58626094HCID 58626094、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

To a solution of 3-chloro-4-methoxy acetophenone (3.0 g, 16.30 mmol) in DMF (15 mL) was added 60% NaH [0.717 g (0.430 g, 17.93 mmol)] at 0° C. under a nitrogen atmosphere. The mixture was stirred for 30 min and a solution of nicotinic acid ethyl ester (2.95 g, 19.56 mmol) in DMF (10 mL) was added slowly to it. The mixture was stirred at temperature in the range of 20-40° C. for 12 hour. It was then poured into ice-cold water (100 mL) and stirred for 15 minutes. The solid was filtered and dried to give the desired compound.

後処理

  1. stirringThe mixture was stirred at temperature in the range of 20-40° C. for 12 hour
  2. stirringstirred for 15 minutes
  3. filtrationThe solid was filtered
  4. customdried

出典と根拠

ORDレコード
ord-1fe0fc5df7554c94bef352c71a8b9a7d
出典データセット
uspto-grants-2010_10
特許番号
US07820654B2

関連ノート

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