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Chlorosuccinimide → HCID 19597513, 화합물

HRID 611535
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HRID 611535 반응식
[NH2:1][C:2]1[C:3]2[C:10]([C:11]3[CH:16]=[CH:15][C:14]([O:17][C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=4)=[CH:13][CH:12]=3)=[CH:9][N:8]([C:24]([CH3:27])([CH3:26])[CH3:25])[C:4]=2[N:5]=[CH:6][N:7]=1.[Cl:28]N1C(=O)CCC1=O>ClCCl>[C:24]([N:8]1[C:4]2[N:5]=[CH:6][N:7]=[C:2]([NH2:1])[C:3]=2[C:10]([C:11]2[CH:12]=[CH:13][C:14]([O:17][C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[CH:15][CH:16]=2)=[C:9]1[Cl:28])([CH3:27])([CH3:26])[CH3:25]
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참가 물질

4

반응물 2

HCID 31398ChlorosuccinimideHCID 99506787-tert-Butyl-5-(4-phenoxy-phenyl)-7H-pyrrolo[2,3-d]pyrimidin-4-ylamine

생성물 1

HCID 19597513HCID 19597513, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of 4-amino-5-(4-phenoxyphenyl)-7-(tert-butyl)pyrrolo[2,3-d]-pyrimidine (0.20 g), N-chlorosuccinimide (80 mg) and dichloromethane (5 ml) was stirred at ambient temperature for 18 hours. The mixture was concentrated under reduced pressure and the residue was partitioned between ethyl acetate and water. The organic layer was separated, dried and evaporated to give an oil which was purified by flash column chromatography on silica using ethyl acetate/triethylamine (95:5) as the mobile phase. Appropriate fractions were collected, combined and evaporated to give 7-(tert-butyl)-6-chloro-5-(4-phenoxyphenyl)-7H-pyrrolo-[2,3-d]pyrimidin-4-ylamine, m.p. 136.8-137.8° C.

후처리

  1. concentrationThe mixture was concentrated under reduced pressure
  2. customthe residue was partitioned between ethyl acetate and water
  3. customThe organic layer was separated
  4. customdried
  5. customevaporated
  6. customto give an oil which
  7. customwas purified by flash column chromatography on silica
  8. customAppropriate fractions were collected
  9. customevaporated

출처 및 근거

ORD 기록
ord-b5fc4b5d592b4da4a2699470e4f40590
출처 데이터셋
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06001839

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