Cyanamide → 3,4-methylenedioxyphenyl-ONN-azoxycyanide

HRID 2259826

반응식

HRID 2259826 반응식
[CH2:1]1[O:9][C:8]2[CH:7]=[CH:6][C:5]([N:10]=[O:11])=[CH:4][C:3]=2[O:2]1.[N:12]#[C:13][NH2:14].BrN1C(=O)CCC1=O>ClCCl>[CH2:1]1[O:9][C:8]2[CH:7]=[CH:6][C:5]([N+:10](=[N:14][C:13]#[N:12])[O-:11])=[CH:4][C:3]=2[O:2]1

참가 물질

5

반응물 3

HCID 9864CyanamideHCID 67184N-bromobutanimideHCID 190017645-Nitroso-1,3-benzodioxole

생성물 1

HCID 117011753,4-methylenedioxyphenyl-ONN-azoxycyanide수율 83.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

3,4-Methylenedioxynitrosobenzene (1.05 g, 6.9 mmol) was dissolved in dichloromethane (20 ml). After the addition of cyanamide (0.42 g, 9.9 mmol) and N-bromosuccinimide (1.8 g, 9.9 mmol) the mixture was stirred at ambient temperature overnight. The resulting mixture was filtered and evaporated to dryness. Column chromatography on silica using 1:1 petroleum ether: ethyl acetate as eluant yielded 1.1 g 3,4-methylenedioxyphenyl-ONN-azoxycyanide as a yellow solid, m.pt. 145°-147° C. (Yield: 82.7% of theoretical).

후처리

  1. filtrationThe resulting mixture was filtered
  2. customevaporated to dryness

출처 및 근거

ORD 기록
ord-590d1a16dbfb420b97f8470cb3495b0f
출처 데이터셋
uspto-grants-1995_12
특허 번호
US05475093

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