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Sodium Carbonate → HCID 21328862, 화합물

HRID 614302
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HRID 614302 반응식
[OH:1][C:2]([CH3:23])([CH2:18][CH2:19][CH2:20][CH2:21][CH3:22])/[CH:3]=[CH:4]/[CH:5]1[CH2:7][C:6]1([C:13]([O:15][CH2:16][CH3:17])=[O:14])[C:8]([O:10][CH2:11][CH3:12])=[O:9].O.[C:25]1(C)C=[CH:29][C:28](S(O)(=O)=O)=[CH:27][CH:26]=1.C([O-])([O-])=[O:37].[Na+].[Na+]>O1C=CCCC1>[O:37]1[CH2:29][CH2:28][CH2:27][CH2:26][CH:25]1[O:1][C:2]([CH3:23])([CH2:18][CH2:19][CH2:20][CH2:21][CH3:22])/[CH:3]=[CH:4]/[CH:5]1[CH2:7][C:6]1([C:8]([O:10][CH2:11][CH3:12])=[O:9])[C:13]([O:15][CH2:16][CH3:17])=[O:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 521998p-Toluenesulfonic acid monohydrateHCID 21328844HCID 21328844, 화합물

생성물 1

HCID 21328862HCID 21328862, 화합물

시약·촉매·용매 1

HCID 80803,4-dihydro-2H-pyran용매

실험 절차

A solution of diethyl trans-2-(3-hydroxy-3-methyl-1-octenyl)cyclopropane-1,1-dicarboxylate (22.4 g), described in Example 31, dihydropyran (80 ml, distilled over sodium) and p-toluenesulfonic acid monohydrate (300 mg) is allowed to stand at room temperature for 30 min. After adding a few ml of 10% Na2CO3 solution the mixture is extracted with ether. The ether extract is washed with water, dried (Na2SO4) and evaporated. Purification of the residue by chromatography on silica gel gives the title compound, nmr (CDCl3) δ 0.87 (t, 3H), 2.48 (m, 1H), 4.6 (1H), 5.5 (m, 2H).

후처리

  1. extractionis extracted with ether
  2. extractionThe ether extract
  3. washis washed with water
  4. dry with materialdried (Na2SO4)
  5. customevaporated
  6. customPurification of the residue by chromatography on silica gel

출처 및 근거

ORD 기록
ord-d0687c0d0c1b46de99699c46e7f3fe8b
출처 데이터셋
uspto-grants-1979_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04144251

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