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Ethyl chloroformate → HCID 22996008, 화합물

HRID 1167466
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HRID 1167466 반응식
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([N:9]2[CH:13]=[CH:12][C:11]([C:14]#[N:15])=[CH:10]2)=[C:6]([F:8])[CH:7]=1.Cl[C:17]([O:19][CH2:20][CH3:21])=[O:18]>N1C=CC=CC=1>[CH2:20]([O:19][C:17]([NH:1][C:2]1[CH:3]=[CH:4][C:5]([N:9]2[CH:13]=[CH:12][C:11]([C:14]#[N:15])=[CH:10]2)=[C:6]([F:8])[CH:7]=1)=[O:18])[CH3:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 10928Ethyl chloroformateHCID 229961405-Amino-2-(3-cyano-1-pyrrolyl)fluorobenzene

생성물 1

HCID 22996008HCID 22996008, 화합물수율 78.3%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

5-Amino-2-(3-cyano-1-pyrrolyl)fluorobenzene (4.6 g, 22.9 mmol) was stirred in dry pyridine (50 ml) 0°. Ethyl chloroformate (2.66 g, 24.5 mmol) was added, and stirring continued for 20 minutes at the same temperature before allowing the temperature to rise to ambient over 2 hours. Solvent was evaporated, the residue treated with iced water (50 ml), filtered off, and dried. Crystallisation of the crude product from ethanol (200 ml) gave the title product (4.9 g) mp 188-190°.

후처리

  1. waitto ambient over 2 hours
  2. customSolvent was evaporated
  3. additionthe residue treated with iced water (50 ml)
  4. filtrationfiltered off
  5. customdried
  6. customCrystallisation of the crude product from ethanol (200 ml)

출처 및 근거

ORD 기록
ord-4eaa8661df40433db41887d4580355e4
출처 데이터셋
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06617339B1

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