Ammonium Chloride → Ici 111075

HRID 224405ノート

反応式

HRID 224405 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 194133Ici 111075

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-20721285dce144de865526e89ff4f2a1
出典データセット
uspto-grants-1980_11
特許番号
US04232032

反応ノート

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