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Oxalyl chloride → 2-Fluorobenzoyl isocyanate

HRID 1004867
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HRID 1004867 반응식
[F:1][C:2]1[CH:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([NH2:6])=[O:5].C(Cl)(=O)[C:12](Cl)=[O:13]>ClCCCl>[F:1][C:2]1[CH:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([N:6]=[C:12]=[O:13])=[O:5]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 65578Oxalyl chlorideHCID 679642-Fluorobenzamide

생성물 1

HCID 130803922-Fluorobenzoyl isocyanate

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

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온도
100 °C

실험 절차

0.47 g (3.0 mmol) of 2-fluorobenzamide and 0.40 g (3.2 mmol, 1.05 eq) of oxalyl chloride were added to 10 ml of 1,2-dichloroethane and then the mixture was stirred for 8 hours at 100° C. The reaction solution was cooled down to room temperature. The reaction solvent and excessive oxalyl chloride were removed by distillation under reduced pressure to obtain 2-fluorobenzoyl isocyanate in an oily state. 10 ml of fresh 1,2-dichloroethane and 0.95 g (3.0 mmol) of 2,4-dibromo-5-trifluoromethyl aniline were successively added thereto, reacted for 2 hours and filtered to obtain 1.11 g (Yield 77%) of the title compound as a solid.

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후처리

  1. temperatureThe reaction solution was cooled down to room temperature
  2. customThe reaction solvent and excessive oxalyl chloride were removed by distillation under reduced pressure

출처 및 근거

ORD 기록
ord-135643e8b5fd4a2ca471d20b5e088051
출처 데이터셋
uspto-grants-2000_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06051737

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