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Dimethyl Sulfoxide → Methyl 8-methylsulfonyl-12-acetoxy-13-(3-trifluoromethylphenoxy)tridecanoate

HRID 328801
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HRID 328801 반응식
[CH3:1][S:2]([C:5](C(OC)=O)([CH2:16][CH2:17][CH2:18][CH:19]([O:32][C:33](=[O:35])[CH3:34])[CH2:20][O:21][C:22]1[CH:27]=[CH:26][CH:25]=[C:24]([C:28]([F:31])([F:30])[F:29])[CH:23]=1)[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12]([O:14][CH3:15])=[O:13])(=[O:4])=[O:3].[Cl-].[Na+].CS(C)=O>O>[CH3:1][S:2]([CH:5]([CH2:16][CH2:17][CH2:18][CH:19]([O:32][C:33](=[O:35])[CH3:34])[CH2:20][O:21][C:22]1[CH:27]=[CH:26][CH:25]=[C:24]([C:28]([F:31])([F:29])[F:30])[CH:23]=1)[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12]([O:14][CH3:15])=[O:13])(=[O:3])=[O:4]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 679Dimethyl SulfoxideHCID 5234Sodium ChlorideHCID 21317568HCID 21317568, 화합물

생성물 1

HCID 21317521Methyl 8-methylsulfonyl-12-acetoxy-13-(3-trifluoromethylphenoxy)tridecanoate수율 190%

시약·촉매·용매 1

HCID 962Water용매

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온도
185 °C

실험 절차

A mixture of methyl 8-methylsulfonyl-8-methoxycarbonyl-12-acetoxy-13-(3-trifluoromethylphenoxy)tridecanoate (5.82 g., 0.01 mole), sodium chloride (0.59 g., 0.01 mole), dimethylsulfoxide (8 ml.), and water (0.2 ml.) is heated in an oil bath at 185° C. for 10 hours under nitrogen. The reaction mixture is then concentrated in vacuo on a steam bath. The dark-colored residue is diluted with water, acidified with 6N hydrochloric acid, and extracted with ether. The ether extracts are washed with water, dried with anhydrous magensium sulfate, and concentrated in vacuo to give the title compound (9.90 g., 0.019 mole, 94%).

후처리

  1. concentrationThe reaction mixture is then concentrated in vacuo on a steam bath
  2. additionThe dark-colored residue is diluted with water
  3. extractionextracted with ether
  4. washThe ether extracts are washed with water
  5. dry with materialdried with anhydrous magensium sulfate
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-d9edf7db857c4561a3f20a10b38f991f
출처 데이터셋
uspto-grants-1977_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04018802

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