Water → 4-ethoxy-5-iodo-7H-pyrrolo[2,3-d]pyrimidine

HRID 1396136ノート

反応式

HRID 1396136 の反応式
[CH2:1]([O:3][C:4]1[C:5]2[CH:12]=[CH:11][NH:10][C:6]=2[N:7]=[CH:8][N:9]=1)[CH3:2].CN(C)C=O.[I:18]N1C(=O)CCC1=O.O>ClCCl>[CH2:1]([O:3][C:4]1[C:5]2[C:12]([I:18])=[CH:11][NH:10][C:6]=2[N:7]=[CH:8][N:9]=1)[CH3:2]

参加物

6

反応物 4

HCID 962WaterHCID 6228DimethylformamideHCID 120273N-IodosuccinimideHCID 579632454-ethoxy-7H-pyrrolo[2,3-d]pyrimidine

生成物 1

HCID 584858444-ethoxy-5-iodo-7H-pyrrolo[2,3-d]pyrimidine収率 95.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To 4-ethoxy-7H-pyrrolo[2,3-d]pyrimidine (11, 1.60 g, 9.8 mmol) in 50.0 mL of dichloromethane, N,N-dimethylformamide (2.0 mL, 26 mmol) and N-iodosuccinimide (2.40 g, 10.7 mmol) are added and the reaction stirred at room temperature for 2 hours. The reaction is poured into water and extracted with ethyl acetate. The organic layer is dried with sodium sulfate, filtered and the filtrate concentrated under vacuum to provide the desired compound (12, 2.70 g).

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialThe organic layer is dried with sodium sulfate
  3. filtrationfiltered
  4. concentrationthe filtrate concentrated under vacuum

出典と根拠

ORDレコード
ord-61521db4c0584885bcec8006230888f5
出典データセット
uspto-grants-2014_12
特許番号
US08901118B2

反応ノート

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