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Sodium Chloride → HCID 44562749, 화합물

HRID 1732436
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HRID 1732436 반응식
COC([C:5]1([CH2:16]/[CH:17]=[CH:18]\[CH2:19][CH3:20])[C:9](=[O:10])[CH:8]=[CH:7][CH:6]1[CH2:11][C:12]([O:14][CH3:15])=[O:13])=O.[Cl-].[Na+]>CS(C)=O.O>[CH3:15][O:14][C:12]([CH2:11][CH:6]1[CH:5]([CH2:16]/[CH:17]=[CH:18]\[CH2:19][CH3:20])[C:9](=[O:10])[CH:8]=[CH:7]1)=[O:13]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 5234Sodium ChlorideHCID 70582387HCID 70582387, 화합물

생성물 1

HCID 44562749HCID 44562749, 화합물수율 91%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매

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온도
175 °C

실험 절차

A 360 mg quantity of 5-methoxycarbonyl-4-methoxycarbonylmethyl-5-(cis-2-pentenyl)-2-cyclopentenone is dissolved in 8 ml of dimethyl sulfoxide containing 23 mg of water. The solution is reacted in a sealed tube with addition of 20 mg of sodium chloride. After the solution has been heated at 175° C. for 4 hours, the product is cooled to room temperature and then extracted with ethyl ether. The ethereal layer is washed, dried and distilled for the removal of the solvent. Purification of the residue by a silica gel column affords a compound (1-a) and compound (1-b) (R2 =CH3 in each). Yield of compound (1-a): 62.5%. Yield of compound (1-b): 28.5%. Combined yield: 91%. B.p. 87°-91° C./2.5 mm Hg.

후처리

  1. temperaturethe product is cooled to room temperature
  2. extractionextracted with ethyl ether
  3. washThe ethereal layer is washed
  4. customdried
  5. distillationdistilled for the removal of the solvent
  6. customPurification of the residue by a silica gel column

출처 및 근거

ORD 기록
ord-21f7b5764c274069828c1b70bffc324a
출처 데이터셋
uspto-grants-1980_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04237308

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