1,1'-Carbonyldiimidazole → 3-(Difluoromethoxy)benzonitrile

HRID 1380048노트

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HRID 1380048 반응식
[F:1][CH:2]([F:13])[O:3][C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][CH:12]=1)[CH:7]=[N:8]O.C1N=CN(C(N2C=NC=C2)=O)C=1>O1CCCC1>[F:1][CH:2]([F:13])[O:3][C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][CH:12]=1)[C:7]#[N:8]

참가 물질

4

반응물 2

HCID 682631,1'-CarbonyldiimidazoleHCID 861304583-(Difluoromethoxy)benzaldehyde Oxime

생성물 1

HCID 27369883-(Difluoromethoxy)benzonitrile수율 54.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 4.95 g of 3-(difluoromethoxy)benzaldehyde oxime in 50 ml of dry tetrahydrofuran was treated with 4.30 g of N,N-carbonyldiimidazole. After the effervescence had subsided, the reaction solution was allowed to stand overnight, then concentrated in vacuo. The residue was taken up in 75 ml of water and the pH adjusted to 4 with hydrochloric acid. The nitrile was extracted into ether, dried over sodium sulfate and concentrated, giving a yellow oil which upon distillation gave 2.45 g of the desired compound as a colorless oil, bp 73°-75° C./0.3 mm.

후처리

  1. concentrationconcentrated in vacuo
  2. extractionThe nitrile was extracted into ether
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated
  5. customgiving a yellow oil which
  6. distillationupon distillation

출처 및 근거

ORD 기록
ord-cb07054d23c2499da774432a83e8dbfd
출처 데이터셋
uspto-grants-1986_04
특허 번호
US04579848

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