Hydrogen Peroxide → HCID 12272042, 화합물

HRID 225151노트

반응식

HRID 225151 반응식
[CH:1](=[C:8]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH3:7].C(=O)(O)[O-:20].[K+].OO>CO>[CH2:2]([CH:1]1[O:20][C:8]1([C:14]([O:16][CH2:17][CH3:18])=[O:15])[C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:3][CH2:4][CH2:5][CH2:6][CH3:7]

참가 물질

5

반응물 3

HCID 784Hydrogen PeroxideHCID 348771Diethyl 2-heptylidenepropanedioateHCID 516893Potassium Bicarbonate

생성물 1

HCID 12272042HCID 12272042, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 31 g of diethyl heptylidenepropanedioate (B. Wojcik and H. Adkins, J. Am. Chem. Soc., 56, 2424 (1934), prepared by the method of A. C. Cope and K. E. Hoyle, J. Am. Chem. Soc., 63, 733 (1941)), 5 g of potassium bicarbonate and 17 g of 30% hydrogen peroxide in 200 ml of methanol was stirred for two hours at 40° C., then allowed to stand at 20° C. for 16 hours. The mixture then was concentrated to 50 ml; 100 ml of water was added and the solution was extracted with two 50-ml volumes of methylene chloride. The solvent was evaporated to give a colorless liquid, which was vacuum distilled to give diethyl 3-hexyloxiranedicarboxylate (2A), bp: 117°-126° C. at 0.1 Torr.

후처리

  1. custom, 56, 2424 (1934), prepared by the method of A
  2. concentrationThe mixture then was concentrated to 50 ml
  3. addition100 ml of water was added
  4. extractionthe solution was extracted with two 50-ml volumes of methylene chloride
  5. customThe solvent was evaporated
  6. customto give a colorless liquid, which
  7. distillationdistilled

출처 및 근거

ORD 기록
ord-29d097ad048d4d0a9603adf09c781b42
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04235923

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