Hydrogen Peroxide → HCID 178429771, 화합물

HRID 1419810노트

반응식

HRID 1419810 반응식
[CH3:1][C:2]1([CH:5]2[CH2:10][CH2:9][C:8](=[O:11])[CH2:7][CH2:6]2)[CH2:4][CH2:3]1.CCC(C)[BH-](C(C)CC)C(C)CC.[Li+].[OH-].[Na+].OO>C1COCC1.C(O)C.O>[CH3:1][C:2]1([C@@H:5]2[CH2:10][CH2:9][C@H:8]([OH:11])[CH2:7][CH2:6]2)[CH2:3][CH2:4]1

참가 물질

8

반응물 4

HCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 3611392Lithium tri-s-butylborohydrideHCID 541016014-(1-Methylcyclopropyl)cyclohexanone

생성물 1

HCID 178429771HCID 178429771, 화합물

시약·촉매·용매 3

HCID 702Ethanol용매HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 4.0 g (26.3 mmol) of 4-(1-methylcyclopropyl)cyclohexanone in 30 ml of THF was added dropwise at -78° C. to 5.5 g (29.0 mmol) of L-Selectride (1M in THF) and the mixture was subsequently stirred for 3 hours. It was then heated to room temperature, and 4 ml of H2O, 15 ml of ethanol, 11 ml of 6N NaOH and 13 ml of 35% strength H2O2 solution were added in succession to the reaction solution. This solution was left to stand overnight and then subjected to aqueous workup. Extraction was carried out with methylene chloride, and the extract was dried and concentrated. 3.4 g (86% of theory) were obtained of a colorless crystal powder, m.p.: 56° to 57° C.

후처리

  1. waitThis solution was left
  2. waitto stand overnight
  3. extractionExtraction
  4. customthe extract was dried
  5. concentrationconcentrated
  6. custom3.4 g (86% of theory) were obtained of a colorless crystal powder, m.p.: 56° to 57° C.

출처 및 근거

ORD 기록
ord-52ab13d1969b4553b3185ba39d940fd3
출처 데이터셋
uspto-grants-1999_03
특허 번호
US05889012

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