Potassium Persulfate → HCID 10707356, 화합물

HRID 1018661노트

반응식

HRID 1018661 반응식
[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

참가 물질

6

반응물 3

HCID 24412Potassium PersulfateHCID 18373917Acetonitrile--water (1/1)HCID 18401890HCID 18401890, 화합물

생성물 1

HCID 10707356HCID 10707356, 화합물

시약·촉매·용매 2

HCID 24463Copper sulfate pentahydrate촉매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-98b3c83bdfca401090720dcf112d2839
출처 데이터셋
uspto-grants-2002_11
특허 번호
US06482852B2

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