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Peracetic Acid → 2,6,6-Trimethyl-1-[1-hydroxy-3-butenyl]-1,2-epoxycyclohexane

HRID 1283359
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HRID 1283359 반응식
C(OO)(=[O:3])C.C([O-])(=O)C.[Na+].[CH3:11][C:12]1[CH2:17][CH2:16][CH2:15][C:14]([CH3:19])([CH3:18])[C:13]=1[CH:20]([OH:24])[CH2:21][CH:22]=[CH2:23].C([O-])([O-])=O.[Na+].[Na+]>O.C(Cl)Cl>[CH3:11][C:12]12[O:3][C:13]1([CH:20]([OH:24])[CH2:21][CH:22]=[CH2:23])[C:14]([CH3:18])([CH3:19])[CH2:15][CH2:16][CH2:17]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6585Peracetic AcidHCID 10340Sodium CarbonateHCID 517045Sodium Acetate2회HCID 124203212,6,6-Trimethyl-1-(1-hydroxy-3-butenyl)-1-cyclohexene

생성물 1

HCID 144665862,6,6-Trimethyl-1-[1-hydroxy-3-butenyl]-1,2-epoxycyclohexane

시약·촉매·용매 2

HCID 962Water
용매
HCID 6344Dichloromethane용매

실험 절차

A mixture of 40 % peracetic acid (105 g.) and anhydrous sodium acetate (3.0 g.) was added at 25° with stirring to a suspension of 2,6,6-trimethyl-1-[1-hydroxy-3-butenyl]-1-cyclohexene (97g.) and anhyd. sodium acetate (60 g.) in 175 ml. of CH2Cl2 (1.5 h.). Stirring was continued for one night and 500 ml. of water were then added to the reaction mixture. The organic layer was separated and, after the usual treatments, distilled to give 98 g. (83 %) of two diastereoisomers of the epoxy product. V.p.c. enabled the separation of the two isomers (Carbowax, 170°, 3 m)

후처리

  1. additionwas added at 25°
  2. waitwas continued for one night
  3. customThe organic layer was separated
  4. distillationafter the usual treatments, distilled
  5. customto give 98 g
  6. customthe separation of the two isomers (Carbowax, 170°, 3 m)

출처 및 근거

ORD 기록
ord-8aab5ecd46a64c0cafd13fd9fac7ba8f
출처 데이터셋
uspto-grants-1976_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03975310

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