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Water → 4-azido-6-cyano-3,4-dihydro-2,2-dimethyl-2H-1-benzopyran

HRID 344771
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반응식

HRID 344771 반응식
Cl[CH:2]1[C:7]2[CH:8]=[C:9]([C:12]#[N:13])[CH:10]=[CH:11][C:6]=2[O:5][C:4]([CH3:15])([CH3:14])[CH2:3]1.[N-:16]=[N+:17]=[N-:18].[Na+].O>CN(C)C=O>[N:16]([CH:2]1[C:7]2[CH:8]=[C:9]([C:12]#[N:13])[CH:10]=[CH:11][C:6]=2[O:5][C:4]([CH3:15])([CH3:14])[CH2:3]1)=[N+:17]=[N-:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 33557Sodium AzideHCID 537676584-Chloro-6-cyano-3,4-dihydro-2,2-dimethyl-2H-1-benzopyran

생성물 1

HCID 101051694-azido-6-cyano-3,4-dihydro-2,2-dimethyl-2H-1-benzopyran

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 4-chloro-6-cyano-3,4-dihydro-2,2-dimethyl-2H-1-benzopyran(3g) and sodium azide (0.9g) in N,N-dimethylformamide (20 ml) was stirred for 3 days at room temperature. Water was added and the mixture extracted with ethyl acetate, the organic phase was separated and further washed with water, then dried over anhydrous sodium sulphate. Filtration and evaporation of the solvent in vacuo gave the title compound (3.03g) as a solid, which was used in the next step without further purification.

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후처리

  1. extractionthe mixture extracted with ethyl acetate
  2. customthe organic phase was separated
  3. washfurther washed with water
  4. dry with materialdried over anhydrous sodium sulphate
  5. filtrationFiltration and evaporation of the solvent in vacuo

출처 및 근거

ORD 기록
ord-ff09516856ad47beb0c09010e4f766a7
출처 데이터셋
uspto-grants-1991_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05053427

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