Potassium Persulfate → HCID 10707356、化合物

HRID 1018661ノート

反応式

HRID 1018661 の反応式
[CH:1]1([CH2:7][O:8][C:9]2[CH:10]=[CH:11][C:12]3[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14][C:13]=3[CH:19]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.S(OOS([O-])(=O)=O)([O-])(=O)=[O:21].[K+].[K+].CC#N.O>O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Cu+2]>[CH:1]1([CH2:7][O:8][C:9]2[CH:10]=[CH:11][C:12]3[C:18](=[O:21])[CH2:17][CH2:16][CH2:15][CH2:14][C:13]=3[CH:19]=2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

参加物

6

反応物 3

HCID 24412Potassium PersulfateHCID 18373917Acetonitrile--water (1/1)HCID 18401890HCID 18401890、化合物

生成物 1

HCID 10707356HCID 10707356、化合物

試薬・触媒・溶媒 2

HCID 24463Copper sulfate pentahydrate触媒HCID 962Water溶媒

実験手順

A mixture of 2-cyclohexylmethoxy-6,7,8,9-tetrahydro-5H-benzocycloheptene (0.50 g, 1.94 mmol), potassium persulfate (1.57 g, 5.82 mmol), copper(II) sulfate pentahydrate (0.48 g, 1.94 mmol) and CH3CN/H2O (1:1, 13 mL) were heated at reflux for 45 min. After cooling the mixture was diluted with water and extracted with EtOAc. The combined extracts were washed with water, dried over magnesium sulfate, concentrated, and chomatographed over silica gel (20% EtOAc/hexane) to a white solid (0.46 g, 87%). MS [M+H]+ 273, m.p. 86-88° C.

後処理

  1. temperaturewere heated
  2. temperatureat reflux for 45 min
  3. temperatureAfter cooling the mixture
  4. extractionextracted with EtOAc
  5. washThe combined extracts were washed with water
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-98b3c83bdfca401090720dcf112d2839
出典データセット
uspto-grants-2002_11
特許番号
US06482852B2

反応ノート

読み込み中…