Iodine → 6-Bromo-3-iodopyrazolo[1,5-a]pyrimidine

HRID 1255862ノート

反応式

HRID 1255862 の反応式
[Br:1][C:2]1[CH:3]=[N:4][C:5]2[N:6]([N:8]=[CH:9][CH:10]=2)[CH:7]=1.[I:11]I>C(#N)C>[Br:1][C:2]1[CH:3]=[N:4][C:5]2[N:6]([N:8]=[CH:9][C:10]=2[I:11])[CH:7]=1

参加物

4

反応物 2

HCID 807IodineHCID 222367016-Bromopyrazolo[1,5-a]pyrimidine

生成物 1

HCID 568452436-Bromo-3-iodopyrazolo[1,5-a]pyrimidine

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of compound 6-bromopyrazolo[1,5-a]pyrimidine (1 eq), ceric ammonium nitrate (0.6 eq), and I2 (0.6 eq) in acetonitrile (10 mL) was stirred over a period of 24 h at room temperature. The formed precipitate was filtered off, washed with acetonitrile, and recrystallized from acetonitrile. The filtrate was evaporated, and the product was extracted with dichloromethane. The latter was evaporated, and the residue was recrystallized from acetonitrile to give 6-bromo-3-iodopyrazolo[1,5-a]pyrimidine.

後処理

  1. filtrationThe formed precipitate was filtered off
  2. washwashed with acetonitrile
  3. customrecrystallized from acetonitrile
  4. customThe filtrate was evaporated
  5. extractionthe product was extracted with dichloromethane
  6. customThe latter was evaporated
  7. customthe residue was recrystallized from acetonitrile

出典と根拠

ORDレコード
ord-fbf98b2bcc1e45488a6c9440734e81bf
出典データセット
uspto-grants-2013_06
特許番号
US08461162B2

反応ノート

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