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

HRID 1396136노트

반응식

HRID 1396136 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-61521db4c0584885bcec8006230888f5
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08901118B2

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