Ammonium Chloride → HCID 178478471、化合物

HRID 224406ノート

反応式

HRID 224406 の反応式
[C:1]([C:3]1[CH:4]=[CH:5][C:6]2[O:11][CH:10]([C:12]([Cl:15])([Cl:14])[Cl:13])[O:9][CH:8]([C:16]([Cl:19])([Cl:18])Cl)[C:7]=2[CH:20]=1)#[N:2].[Cl-].[NH4+].[N-:23]=[N+:24]=[N-:25].[Na+]>CN(C)C=O>[Cl:18][C:16]([Cl:19])=[C:8]1[C:7]2[CH:20]=[C:3]([C:1]3[NH:25][N:24]=[N:23][N:2]=3)[CH:4]=[CH:5][C:6]=2[O:11][CH:10]([C:12]([Cl:13])([Cl:14])[Cl:15])[O:9]1

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 233329632,4-Bis(trichloromethyl)-2H,4H-1,3-benzodioxine-6-carbonitrile

生成物 1

HCID 178478471HCID 178478471、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 6-cyano-2,4-bis(trichloromethyl)benzo[1,3]dioxin (1.98 g.), ammonium chloride (0.33 g.) and sodium azide in anhydrous dimethylformamide was warmed on the steam bath for 16 hours. The reaction mixture was cooled, poured onto ice and kept for 16 hours. The amorphous white product was filtered off, triturated with acetic acid, and crystallised from chloroform to give 4-dichloromethylene-6-(tetrazol-5-yl)-2-trichloromethylbenzo[1,3]dioxin, m.p. 222° 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 amorphous white product was filtered off
  5. customtriturated with acetic acid
  6. customcrystallised from chloroform

出典と根拠

ORDレコード
ord-03e5f3dcdc014a4f9a1b26ebd567e47f
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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