Ammonium Chloride → Ici 111075

HRID 224405노트

반응식

HRID 224405 반응식
[Cl:1][C:2]([Cl:21])([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]([OH:19])=[O:18])[CH:15]=[CH:16][C:5]=2[O:4]1.[Cl-].[NH4+].[N-]=[N+]=[N-].[Na+]>CS(C)=O>[Cl:11][C:9]([Cl:10])=[C:7]1[C:6]2[CH:13]=[C:14]([C:17]([OH:19])=[O:18])[CH:15]=[CH:16][C:5]=2[O:4][CH:3]([C:2]([Cl:1])([Cl:21])[Cl:20])[O:8]1

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 1941342,4-Bis(trichloromethyl)-2H,4H-1,3-benzodioxine-6-carboxylic acid

생성물 1

HCID 194133Ici 111075

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

A mixture of 2,4-bis(trichloromethyl)benzo[1,3]dioxin-6-carboxylic acid (2.08 g.), ammonium chloride (0.33 g.) and sodium azide (0.36 g.) in anhydrous dimethylsulphoxide (10 ml.) was warmed on the steam bath for 16 hours. The reaction mixture was cooled, poured onto ice and kept for 16 hours. The white product was filtered off, washed with water and dried, and crystallised from aqueous ethanol to give 4-dichloromethylene-2-trichloromethybenzo[1,3]dioxin-6-carboxylic acid, m.p. 222°-223° C.

후처리

  1. temperaturewas warmed on the steam bath for 16 hours
  2. temperatureThe reaction mixture was cooled
  3. additionpoured onto ice
  4. filtrationThe white product was filtered off
  5. washwashed with water
  6. customdried
  7. customcrystallised from aqueous ethanol

출처 및 근거

ORD 기록
ord-20721285dce144de865526e89ff4f2a1
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04232032

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