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

HRID 2116461ノート

反応式

HRID 2116461 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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

後処理

  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

出典と根拠

ORDレコード
ord-863f109b2823438793626974aaa0fe92
出典データセット
uspto-grants-2008_10
特許番号
US07439240B2

反応ノート

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