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

HRID 485438ノート

反応式

HRID 485438 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-24e50a0680304f97a73d4bb42a8af988
出典データセット
uspto-grants-1985_08
特許番号
US04536507

反応ノート

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