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2,4-Bis(trichloromethyl)-2H,4H-1,3-benzodioxine-6-carboxamide → 2,4-Bis(dichloromethylene)benzo[1,3]dioxin-6-carboxamide

HRID 224407
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반응식

HRID 224407 반응식
[Cl:1][C:2](Cl)([Cl:20])[CH:3]1[O:8][CH:7]([C:9](Cl)([Cl:11])[Cl:10])[C:6]2[CH:13]=[C:14]([C:17]([NH2:19])=[O:18])[CH:15]=[CH:16][C:5]=2[O:4]1.CC(C)([O-])C.[K+]>CS(C)=O>[Cl:20][C:2]([Cl:1])=[C:3]1[O:8][C:7](=[C:9]([Cl:11])[Cl:10])[C:6]2[CH:13]=[C:14]([C:17]([NH2:19])=[O:18])[CH:15]=[CH:16][C:5]=2[O:4]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 233329312,4-Bis(trichloromethyl)-2H,4H-1,3-benzodioxine-6-carboxamideHCID 23665647Potassium tert-butoxide

생성물 1

HCID 233329192,4-Bis(dichloromethylene)benzo[1,3]dioxin-6-carboxamide

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

A mixture of 2,4-bis(trichloromethyl)benzo[1,3]dioxin-6-carboxamide (3.14 g.) and potassium t-butoxide (2.5 g.) in 50% aqueous dimethylsulphoxide (50 ml.) was heated at 80°-90° C. for 2 hours. The solid product was filtered off, dried and crystallised from ethanol to give 2,4-bis(dichloromethylene)benzo[1,3]dioxin-6-carboxamide, m.p. 217°-218° C.

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후처리

  1. temperaturewas heated at 80°-90° C. for 2 hours
  2. filtrationThe solid product was filtered off
  3. customdried
  4. customcrystallised from ethanol

출처 및 근거

ORD 기록
ord-d1c62ccbd39e4b7fbf062e1a479fff8a
출처 데이터셋
uspto-grants-1980_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04232032

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