Sodium hydride → HCID 58626094, 화합물

HRID 1161696

반응식

HRID 1161696 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 58626094HCID 58626094, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1fe0fc5df7554c94bef352c71a8b9a7d
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07820654B2

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