Ammonium Chloride → 5-(6-chloro-5,7-dimethyl-4-oxo-4H-1-benzopyran-2-yl) tetrazole

HRID 1580706노트

반응식

HRID 1580706 반응식
[Cl:1][C:2]1[C:3]([CH3:16])=[CH:4][C:5]2[O:10][C:9]([C:11]#[N:12])=[CH:8][C:7](=[O:13])[C:6]=2[C:14]=1[CH3:15].[N-:17]=[N+:18]=[N-:19].[Na+].[Cl-].[NH4+]>CN(C)C=O>[Cl:1][C:2]1[C:3]([CH3:16])=[CH:4][C:5]2[O:10][C:9]([C:11]3[NH:19][N:18]=[N:17][N:12]=3)=[CH:8][C:7](=[O:13])[C:6]=2[C:14]=1[CH3:15]

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 213926006-chloro-5,7-dimethyl-4-oxo-4H-1-benzopyran-2-carbonitrile

생성물 1

HCID 1784223865-(6-chloro-5,7-dimethyl-4-oxo-4H-1-benzopyran-2-yl) tetrazole

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 23.4 parts of 6-chloro-5,7-dimethyl-4-oxo-4H-1-benzopyran-2-carbonitrile, 7.8 parts of sodium azide, 6.4 parts of ammonium chloride and 200 parts of N,N-dimethylformamide was stirred and heated on the steam bath for 18 hours. Most of the solvent was then removed by distillation under reduced pressure. A solution of the residue in 400 parts of water was acidified with 20% hydrochloric acid. The precipitated solid was filtered off, washed with water and crystallised from dioxan to give 15.5 parts of 5-(6-chloro-5,7-dimethyl-4-oxo-4H-1-benzopyran-2-yl) tetrazole as a colourless solid, melting point 246°-247°C (decomposition).

후처리

  1. temperatureheated on the steam bath for 18 hours
  2. customMost of the solvent was then removed by distillation under reduced pressure
  3. filtrationThe precipitated solid was filtered off
  4. washwashed with water
  5. customcrystallised from dioxan

출처 및 근거

ORD 기록
ord-9afbc88ccfd644a8ac5a6592c88118d8
출처 데이터셋
uspto-grants-1976_01
특허 번호
US03933845

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