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Pyridine → HCID 13335393, 화합물

HRID 1981045
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HRID 1981045 반응식
[CH2:1]([CH:4]1[C:8]([OH:10])([CH3:9])[CH:7]=[CH:6][C:5]1=[O:11])[CH:2]=[CH2:3].N1C=CC=CC=1.ClCCl.[C:21](Cl)(=[O:23])[CH3:22]>O>[C:21]([O:10][C:8]1([CH3:9])[CH:7]=[CH:6][C:5](=[O:11])[CH:4]1[CH2:1][CH:2]=[CH2:3])(=[O:23])[CH3:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 1049PyridineHCID 6344DichloromethaneHCID 6367Acetyl chloride2회HCID 128798724-Hydroxy-4-methyl-5-(prop-2-en-1-yl)cyclopent-2-en-1-one

생성물 1

HCID 13335393HCID 13335393, 화합물수율 94.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Into a flask equipped with a stirrer and a thermometer, dl-2-allyl-3-hydroxy-3-methyl-4-cyclopentenone (30.4 g), pyridine (30 g) and dichloromethane (300 g) were charged, and acetyl chloride (30 g) was dropwise added thereto at a temperature from 10° to 20° C. in 2 hours. Then, stirring was continued at a room temperature for 24 hours. To the reaction mixture kept below 10° C., water (100 ml) was added to decompose excess of acetyl chloride. From the resultant mixture, the organic layer was separated and washed with 1% hydrochloric acid, 1% sodium bicarbonate solution and water in order. Removal of the solvent by distillation gave dl-3-acetoxy-2-allyl-3-methyl-4-cyclopentenone (36.5 g). Yield, 94%.

후처리

  1. customInto a flask equipped with a stirrer
  2. waitwas continued at a room temperature for 24 hours
  3. customkept below 10° C.
  4. customFrom the resultant mixture, the organic layer was separated
  5. washwashed with 1% hydrochloric acid, 1% sodium bicarbonate solution and water in order
  6. customRemoval of the solvent
  7. distillationby distillation

출처 및 근거

ORD 기록
ord-1dd76370304e4e2db59841bb2d7d4c34
출처 데이터셋
uspto-grants-1985_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04511655

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