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Chloromethyl Methyl Ether → HCID 53991562, 화합물

HRID 637325
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HRID 637325 반응식
[H-].[Li+].[CH3:3][C:4]1([CH3:12])[C@H:6]([CH:7]=[O:8])[C@H:5]1[C:9]([OH:11])=[O:10].[CH3:13][O:14][CH2:15]Cl.C(=O)(O)[O-].[Na+]>O.O1CCCC1>[CH3:3][C:4]1([CH3:12])[C@H:6]([CH:7]=[O:8])[C@H:5]1[C:9]([O:11][CH2:13][O:14][CH3:15])=[O:10]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 7864Chloromethyl Methyl EtherHCID 62714Lithium hydrideHCID 516892Sodium BicarbonateHCID 12919118(1R,trans) 2,2-dimethyl-3-formyl-cyclopropane-carboxylic acid

생성물 1

HCID 53991562HCID 53991562, 화합물수율 45.2%

시약·촉매·용매 2

HCID 962Water
용매
HCID 8028Tetrahydrofuran용매

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온도
15 °C

실험 절차

A mixture of 1.64 g of lithium hydride and 25.6 g of (1R,trans) 2,2-dimethyl-3-formyl-cyclopropane-carboxylic acid and 25 ml of tetrahydrofuran was stirred at 15° C. for 30 minutes and then 18.2 g of a freshly prepared chloromethyl methyl ether (0.225 mols) were added thereto. The mixture was stirred at 20° C. for 4 hours and was then poured into a mixture of ice, water and sodium bicarbonate with stirring. The mixture was extracted with isopropyl ether and the organic phase was evaporated to dryness under reduced pressure. The residue was rectified under vacuum to obtain 15.15 g of methoxymethyl (1R,trans) 2,2-dimethyl-3-formyl-cyclopropane-carboxylate with a boiling point of 67° C. at 0.05 mm Hg.

후처리

  1. stirringThe mixture was stirred at 20° C. for 4 hours
  2. stirringwith stirring
  3. extractionThe mixture was extracted with isopropyl ether
  4. customthe organic phase was evaporated to dryness under reduced pressure

출처 및 근거

ORD 기록
ord-f727421f4ed148d2b30f4fd2c1123eff
출처 데이터셋
uspto-grants-1985_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04556666

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