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Dichloromaleic anhydride → HCID 13073055, 화합물

HRID 1263052
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HRID 1263052 반응식
[Cl:1][C:2]1[C:3]([O:5][C:6](=[O:9])[C:7]=1[Cl:8])=O.[F:10][CH:11]([F:20])[O:12][C:13]1[CH:14]=[C:15]([CH:17]=[CH:18][CH:19]=1)[NH2:16]>O1CCOCC1>[Cl:8][C:7]1[C:6]([N:16]([C:15]2[CH:17]=[CH:18][CH:19]=[C:13]([O:12][CH:11]([F:10])[F:20])[CH:14]=2)[C:3](=[O:5])[C:2]=1[Cl:1])=[O:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 70728Dichloromaleic anhydrideHCID 27741103-(Difluoromethoxy)aniline

생성물 1

HCID 13073055HCID 13073055, 화합물수율 95%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

16.7 g (0.1 mole) of 2,3-dichloromaleic anhydride is dissolved in 100 ml of dioxane, and a solution of 15.9 g (0.1 mole) of m-difluoromethoxyaniline in 30 ml of dioxane is added dropwise to it at room temperature over 20 minutes with stirring. Thereafter, the resulting solution is stirred at 70°-80° C. for 2 hours and the dioxane is then distilled off under a reduced pressure. Water is added to the residue to precipitate crystals. The precipitated crystals are filtered off and recrystallized to give 29.2 g (yield: 95%) of 2,3-dichloro-N-(m-difluoromethoxyphenyl)maleimide melting at 122°-124° C. in the form of light yellow plate crystals.

후처리

  1. stirringThereafter, the resulting solution is stirred at 70°-80° C. for 2 hours
  2. distillationthe dioxane is then distilled off under a reduced pressure
  3. additionWater is added to the residue
  4. customto precipitate crystals
  5. filtrationThe precipitated crystals are filtered off
  6. customrecrystallized

출처 및 근거

ORD 기록
ord-659000ad08e947b78939a449b6b7d3b9
출처 데이터셋
uspto-grants-1984_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04455315

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