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

HRID 82253

反応式

HRID 82253 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 148092816-Chloro-7-iodo-7-deazapurine収率 79%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2c94fdeb27714705b957ca8d9de3bb7e
出典データセット
uspto-grants-2014_09
特許番号
US08846698B2

関連ノート

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