m-Chloroperbenzoic acid → HCID 13645908、化合物

HRID 1982171ノート

反応式

HRID 1982171 の反応式
ClC1C=CC=C(C(OO)=[O:9])C=1.[CH3:12][N:13]1[C:18]([O:19][C:20]2[CH:25]=[CH:24][CH:23]=[C:22]([CH3:26])[CH:21]=2)=[N:17][S:16](=[O:27])[N:15]=[C:14]1[O:28][C:29]1[CH:34]=[CH:33][CH:32]=[C:31]([CH3:35])[CH:30]=1>C(Cl)(Cl)Cl.C(Cl)Cl>[CH3:12][N:13]1[C:18]([O:19][C:20]2[CH:25]=[CH:24][CH:23]=[C:22]([CH3:26])[CH:21]=2)=[N:17][S:16](=[O:9])(=[O:27])[N:15]=[C:14]1[O:28][C:29]1[CH:34]=[CH:33][CH:32]=[C:31]([CH3:35])[CH:30]=1

参加物

5

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 13645907HCID 13645907、化合物

生成物 1

HCID 13645908HCID 13645908、化合物

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒2 回HCID 6344Dichloromethane溶媒

実験手順

A solution of m-chloroperbenzoic acid (4.7 g) in chloroform (30 ml) is added at RT to a stirred solution of 4-methyl-3,5-bis-(3-methylphenoxy)1,2,4,6-thiatriazine-1-oxide (3.1 g) in chloroform (15 ml). The reaction mixture is refluxed for about 5 minutes and the precipitate taken up in methylene chloride, washed with sat'd aq. Na2CO3, brine, dried, filtered and evaporated to a solid. The solid is recrystallized from isopropyl acetate using charcoal, affording the desired product, M.P.=221°-223° C.

後処理

  1. temperatureThe reaction mixture is refluxed for about 5 minutes
  2. washwashed with sat'd aq. Na2CO3, brine
  3. customdried
  4. filtrationfiltered
  5. customevaporated to a solid
  6. customThe solid is recrystallized from isopropyl acetate

出典と根拠

ORDレコード
ord-893df80bb3f44ebdb2bbfeccab2d4421
出典データセット
uspto-grants-1986_06
特許番号
US04595683

反応ノート

読み込み中…