Ammonium Chloride → HCID 178478471, 화합물

HRID 224406노트

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HRID 224406 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 178478471HCID 178478471, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-03e5f3dcdc014a4f9a1b26ebd567e47f
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04232032

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