Hydrochloric Acid → HCID 68525961, 화합물

HRID 884110노트

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HRID 884110 반응식
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([O:8][C:9]2[CH:14]=[CH:13][C:12]([CH2:15][CH2:16][C:17]([O:19][CH2:20][CH3:21])=[O:18])=[CH:11][C:10]=2[O:22][CH3:23])=[N:6][CH:7]=1.N1C=CC=CC=1.[Cl:30][C:31]1[CH:32]=[C:33]([CH:37]=[CH:38][C:39]=1[Cl:40])[C:34](Cl)=[O:35].Cl>ClCCl>[Cl:30][C:31]1[CH:32]=[C:33]([CH:37]=[CH:38][C:39]=1[Cl:40])[C:34]([NH:1][C:2]1[CH:3]=[CH:4][C:5]([O:8][C:9]2[CH:14]=[CH:13][C:12]([CH2:15][CH2:16][C:17]([O:19][CH2:20][CH3:21])=[O:18])=[CH:11][C:10]=2[O:22][CH3:23])=[N:6][CH:7]=1)=[O:35]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 76403Benzoyl chloride, 3,4-dichloro-HCID 68527029HCID 68527029, 화합물

생성물 1

HCID 68525961HCID 68525961, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Under ice cooling, to a solution of ethyl 3-(4-(5-aminopyridin-2-yloxy)-3-methoxyphenyl)propionate (1.43 g, 4.5 mmol) in dichloromethane (30 mL) was added pyridine (0.44 mL, 5.4 mmol), and then 3,4-dichlorobenzoyl chloride (0.99 g, 4.7 mmol). The resulting solution was stirred for 1 hour under ice cooling, and then for 10 hours at room temperature. To the resulting reaction solution was added 10% hydrochloric acid, and extracted with dichloromethane. The dichloromethane layer was washed with water, dried over anhydrous magnesium sulfate, and evaporated. To the residue was added diethyl ether, and stirred. The precipitates were collected by filtration. After washing with water and diethyl ether, the precipitates were air dried at 60° C., to thereby yield 0.52 g of the title compound.

후처리

  1. waitfor 10 hours at room temperature
  2. customTo the resulting reaction solution
  3. extractionextracted with dichloromethane
  4. washThe dichloromethane layer was washed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customevaporated
  7. additionTo the residue was added diethyl ether
  8. stirringstirred
  9. filtrationThe precipitates were collected by filtration
  10. washAfter washing with water and diethyl ether
  11. customdried at 60° C.

출처 및 근거

ORD 기록
ord-15002a5bcdad469db0d6cf2a8f39fb2b
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08236826B2

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