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2-Bromo-4-fluorobenzene-1-sulfonyl chloride → HCID 66685755, 화합물

HRID 1778402
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인쇄 미리보기

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HRID 1778402 반응식
[Br:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[S:9](Cl)(=[O:11])=[O:10].[NH2:13][C:14]1[C:19]([C:20]([O:22][CH3:23])=[O:21])=[C:18]([NH2:24])[CH:17]=[CH:16][C:15]=1[C:25]1[CH:29]=[CH:28][O:27][C:26]=1[C:30]([O:32][CH2:33][CH3:34])=[O:31]>C(Cl)Cl.N1C=CC=CC=1>[NH2:13][C:14]1[C:19]([C:20]([O:22][CH3:23])=[O:21])=[C:18]([NH:24][S:9]([C:3]2[CH:4]=[CH:5][C:6]([F:8])=[CH:7][C:2]=2[Br:1])(=[O:11])=[O:10])[CH:17]=[CH:16][C:15]=1[C:25]1[CH:29]=[CH:28][O:27][C:26]=1[C:30]([O:32][CH2:33][CH3:34])=[O:31]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 27782162-Bromo-4-fluorobenzene-1-sulfonyl chloride3회HCID 66685481Ethyl 3-(2,4-diamino-3-methoxycarbonylphenyl)-furan-2-carboxylate2회

생성물 1

HCID 66685755HCID 66685755, 화합물수율 83.1%

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 6344Dichloromethane용매

실험 절차

2-Bromo-4-fluorobenzenesulfonyl chloride (0.584 g) was added to a solution of ethyl 3-(2,4-diamino-3-methoxycarbonylphenyl)-furan-2-carboxylate (Intermediate 89, 0.650 g) in DCM (30 mL) and pyridine (10 mL). The resultant mixture was stirred at room temperature for 45 minutes. A further amount of 2-bromo-4-fluorobenzene-sulfonyl chloride (0.584 g) was added and the mixture stirred for a further 1 hour. A further amount of 2-bromo-4-fluorobenzenesulfonyl chloride (0.300 g) was added and the mixture stirred for a further 30 minutes. The mixture was concentrated in vacuo and the residue was partitioned between water and DCM. The organic layer was dried (MgSO4), filtered and the filtrate was concentrated in vacuo. The residue was triturated with methanol and the resultant solid was collected by filtration and air dried to give ethyl 3-[2-amino-4-(2-bromo-4-fluorobenzenesulfonylamino)-3-methoxycarbonylphenyl]-furan-2-carboxylate (0.960 g) as a powder.

후처리

  1. stirringthe mixture stirred for a further 30 minutes
  2. concentrationThe mixture was concentrated in vacuo
  3. customthe residue was partitioned between water and DCM
  4. dry with materialThe organic layer was dried (MgSO4)
  5. filtrationfiltered
  6. concentrationthe filtrate was concentrated in vacuo
  7. customThe residue was triturated with methanol
  8. filtrationthe resultant solid was collected by filtration and air
  9. customdried

출처 및 근거

ORD 기록
ord-e4d3c2ad457545b38b76b2634a8eb6bc
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09266896B2

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