Iodoethane → 4-Chloro-7-ethyl-2-(methylthio)-7H-pyrrolo[2,3-d]pyrimidine

HRID 2116461

반응식

HRID 2116461 반응식
[H-].[Na+].[Cl:3][C:4]1[C:5]2[CH:14]=[CH:13][NH:12][C:6]=2[N:7]=[C:8]([S:10][CH3:11])[N:9]=1.[CH2:15](I)[CH3:16]>CN(C)C=O>[Cl:3][C:4]1[C:5]2[CH:14]=[CH:13][N:12]([CH2:15][CH3:16])[C:6]=2[N:7]=[C:8]([S:10][CH3:11])[N:9]=1

참가 물질

5

반응물 3

HCID 6340IodoethaneHCID 24758Sodium hydrideHCID 53244144-chloro-2-(methylthio)-7H-pyrrolo[2,3-d]pyrimidine

생성물 1

HCID 859081894-Chloro-7-ethyl-2-(methylthio)-7H-pyrrolo[2,3-d]pyrimidine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Sodium hydride (0.44 g, 60% dispersion in oil) was added portionwise to a stirred solution of 4-chloro-2-(methylthio)-7H-pyrrolo[2,3-d]pyrimidine (2 g) in N,N-dimethylformamide (30 ml) at 0° C. After 0.75 h, ethyl iodide (0.88 ml) was added, the mixture stirred for 2 h, quenched with water and partitioned between ethyl acetate and brine. The organics were washed with water, dried (MgSO4), evaporated under reduced pressure and the residue purified by chromatography on silica eluting with 15% ethyl acetate in isohexane. Yield 1.98 g

후처리

  1. customquenched with water
  2. custompartitioned between ethyl acetate and brine
  3. washThe organics were washed with water
  4. dry with materialdried (MgSO4)
  5. customevaporated under reduced pressure
  6. customthe residue purified by chromatography on silica eluting with 15% ethyl acetate in isohexane

출처 및 근거

ORD 기록
ord-863f109b2823438793626974aaa0fe92
출처 데이터셋
uspto-grants-2008_10
특허 번호
US07439240B2

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