N-Iodosuccinimide → 6-Chloro-7-iodo-7-deazapurine

HRID 82253

반응식

HRID 82253 반응식
[Cl:1][C:2]1[C:3]2[CH:10]=[CH:9][NH:8][C:4]=2[N:5]=[CH:6][N:7]=1.[I:11]N1C(=O)CCC1=O>C(Cl)Cl>[Cl:1][C:2]1[C:3]2[C:10]([I:11])=[CH:9][NH:8][C:4]=2[N:5]=[CH:6][N:7]=1

참가 물질

4

반응물 2

HCID 120273N-IodosuccinimideHCID 53566827H-Pyrrolo(2,3-d)pyrimidine, 4-chloro-

생성물 1

HCID 148092816-Chloro-7-iodo-7-deazapurine수율 79%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a suspension of 4-chloro-7H-pyrrolo[2,3-d]pyrimidine (70.5 g, 0.45 mol) in DCM (1.8 L) was added N-iodosuccinimide (120 g, 0.54 mol) in portions. After addition, the mixture was stirred at room temperature overnight. The solid was filtered and washed with water (250 mL), MeOH (280 mL) and CH2Cl2 (280 mL) sequentially. The solid was dried under vacuum to afford 4-chloro-5-iodo-7H-pyrrolo[2,3-d]pyrimidine as a brown solid in 79% yield, 107 g.

후처리

  1. additionAfter addition
  2. filtrationThe solid was filtered
  3. washwashed with water (250 mL), MeOH (280 mL) and CH2Cl2 (280 mL) sequentially
  4. customThe solid was dried under vacuum

출처 및 근거

ORD 기록
ord-2c94fdeb27714705b957ca8d9de3bb7e
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846698B2

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