m-Chloroperbenzoic acid → 3-Cyano-8-nitrodibenzo[b,f]thiepin-5,5-dioxide

HRID 485438노트

반응식

HRID 485438 반응식
[C:1]([C:3]1[CH:4]=[CH:5][C:6]2[CH:12]=[CH:11][C:10]3[CH:13]=[C:14]([N+:17]([O-:19])=[O:18])[CH:15]=[CH:16][C:9]=3[S:8][C:7]=2[CH:20]=1)#[N:2].ClC1C=CC=C(C(OO)=O)C=1.[OH-:32].[Ca+2].[OH-:34]>C(Cl)(Cl)Cl>[C:1]([C:3]1[CH:4]=[CH:5][C:6]2[CH:12]=[CH:11][C:10]3[CH:13]=[C:14]([N+:17]([O-:19])=[O:18])[CH:15]=[CH:16][C:9]=3[S:8](=[O:34])(=[O:32])[C:7]=2[CH:20]=1)#[N:2]

참가 물질

5

반응물 3

HCID 70297m-Chloroperbenzoic acidHCID 6093208Calcium HydroxideHCID 131518793-Cyano-8-nitrodibenzo[b,f]thiepin

생성물 1

HCID 202702143-Cyano-8-nitrodibenzo[b,f]thiepin-5,5-dioxide

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

2 G. 3-cyano-8-nitrodibenzo[b,f]thiepin is dissolved in 600 cc. chloroform and 12 g. m-chloroperbenzoic acid added. The solution is stirred for 24 hours. Excess powdered calcium hydroxide is added, the mixture filtered through celite, the filtrate evaporated to dryness and the residue chromatographed on silica gel. Elution with 5% ethyl acetate in benzene afforded 1.36 g. (61%) of pure sulfone.

후처리

  1. additionis added
  2. filtrationthe mixture filtered through celite
  3. customthe filtrate evaporated to dryness
  4. customthe residue chromatographed on silica gel
  5. washElution with 5% ethyl acetate in benzene
  6. customafforded 1.36 g

출처 및 근거

ORD 기록
ord-24e50a0680304f97a73d4bb42a8af988
출처 데이터셋
uspto-grants-1985_08
특허 번호
US04536507

반응 노트

불러오는 중…