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

HRID 1255862노트

반응식

HRID 1255862 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fbf98b2bcc1e45488a6c9440734e81bf
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08461162B2

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