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1-Bromo-2-Chloroethane → HCID 23504940, 화합물

HRID 1884878
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HRID 1884878 반응식
[OH:1][C:2]1[C:15]2[C:14](=[O:16])[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[S:7][C:6]=2[C:5]([OH:17])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:25][CH2:26][Cl:27]>CC(C)=O>[Cl:27][CH:26]([O:1][C:2]1[C:15]2[C:14](=[O:16])[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[S:7][C:6]=2[C:5]([OH:17])=[CH:4][CH:3]=1)[CH3:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 78491-Bromo-2-ChloroethaneHCID 11430Potassium CarbonateHCID 235049441,4-Dihydroxy-9H-thioxanthen-9-one

생성물 1

HCID 23504940HCID 23504940, 화합물수율 66.4%

시약·촉매·용매 1

HCID 180Acetone용매2회

실험 절차

A solution of 120 mg of 1,4-dihydroxythioxanthone in 100 ml of acetone is stirred for 0.5 h at room temperature with 138 mg of potassium carbonate. A solution of 80 mg of 1-bromo-2-chloroethane in 5 ml of acetone is then added and the mixture refluxed for 24 h. The heterogeneous mixture is cooled, filtered, concentrated under reduced pressure and purified by silica gel column chromatography using a 1:1 mixture of hexanes and ethyl acetate to produce 100 mg of a yellow-red crystals (65%).

후처리

  1. temperaturethe mixture refluxed for 24 h
  2. temperatureThe heterogeneous mixture is cooled
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. custompurified by silica gel column chromatography
  6. additiona 1:1 mixture of hexanes and ethyl acetate

출처 및 근거

ORD 기록
ord-e17a70789d714896aeb530393ec49ea6
출처 데이터셋
uspto-grants-2004_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06767919B2

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