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Potassium Carbonate → Ethyl 3-[[[3-(4-acetyl-3-hydroxy-2-propylphenoxy)-2-hydroxypropyl]thio]methyl]-1-oxa-4-thiaspiro[4.4]nonane-7-acetate

HRID 1608278
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HRID 1608278 반응식
[CH2:1]([C:4]1[C:14]([OH:15])=[C:13]([C:16](=[O:18])[CH3:17])[CH:12]=[CH:11][C:5]=1[O:6][CH2:7][CH:8]1[O:10][CH2:9]1)[CH2:2][CH3:3].[SH:19][CH2:20][CH:21]1[CH2:25]S[C:23]2([CH2:29][CH2:28][CH:27]([CH2:30][C:31]([O:33][CH2:34][CH3:35])=[O:32])[CH2:26]2)[S:22]1.C(=O)([O-])[O-:37].[K+].[K+]>C(C(C)=O)C>[C:16]([C:13]1[CH:12]=[CH:11][C:5]([O:6][CH2:7][CH:8]([OH:10])[CH2:9][S:19][CH2:20][CH:21]2[S:22][C:23]3([CH2:29][CH2:28][CH:27]([CH2:30][C:31]([O:33][CH2:34][CH3:35])=[O:32])[CH2:26]3)[O:37][CH2:25]2)=[C:4]([CH2:1][CH2:2][CH3:3])[C:14]=1[OH:15])(=[O:18])[CH3:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 27752301-(2-Hydroxy-4-(2-oxiranylmethoxy)-3-propylphenyl)ethanoneHCID 19849025Ethyl 2-(mercaptomethyl)-1,4-dithiaspiro[4.4]nonane-7-acetate

생성물 1

HCID 19849026Ethyl 3-[[[3-(4-acetyl-3-hydroxy-2-propylphenoxy)-2-hydroxypropyl]thio]methyl]-1-oxa-4-thiaspiro[4.4]nonane-7-acetate

시약·촉매·용매 1

HCID 6569
Methyl Ethyl Ketone
용매

실험 절차

3-(2-n-Propyl-3-hydroxy-4-acetylphenoxy)-1,2-epoxypropane (1.5 g, 0.006 mol) (described in U.S. Pat. No. 4,565,882) is dissolved in 20 ml of methyl ethyl ketone. To this solution is added the mercaptan of Example G (1.75 g, 0.006 mol) and anhydrous potassium carbonate (2.5 g) and the reaction mixture is refluxed with stirring under a nitrogen atmosphere for 24 hrs. The reaction is cooled to room temperature, filtered and the filtrate is concentrated on a rotary evaporator. The residue is chromatographed on silica gel using mixtures of ethyl acetate and hexane as eluents to give the titled compound.

후처리

  1. temperaturethe reaction mixture is refluxed
  2. filtrationfiltered
  3. concentrationthe filtrate is concentrated on a rotary evaporator
  4. customThe residue is chromatographed on silica gel using mixtures of ethyl acetate and hexane as eluents

출처 및 근거

ORD 기록
ord-2057bcd097f74eca890cf6d2e7e04cfe
출처 데이터셋
uspto-grants-1989_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04870098

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