Water → 1,1-Dimethylethyl 2-chloro-3-methoxymethyloxirane-carboxylate

HRID 2292577

반응식

HRID 2292577 반응식
[CH3:1][O:2][CH2:3][CH:4]=[O:5].Cl[CH:7]([Cl:15])[C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9].CCOCC.O>O1CCCC1>[Cl:15][C:7]1([C:8]([O:10][C:11]([CH3:12])([CH3:13])[CH3:14])=[O:9])[CH:4]([CH2:3][O:2][CH3:1])[O:5]1

참가 물질

6

반응물 4

HCID 962WaterHCID 3283Diethyl EtherHCID 91563MethoxyacetaldehydeHCID 30164831,1-Dimethylethyl dichloroacetate

생성물 1

HCID 214784451,1-Dimethylethyl 2-chloro-3-methoxymethyloxirane-carboxylate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
-20 °C

실험 절차

A mixture of 2.106 g of methoxyacetaldehyde, 3.8 ml of tertbutyl dichloroacetate and 25 ml of tetrahydrofuran was cooled to -20° C. and over 15 minutes, 29 ml of potassium tertbutylate in tetrahydrofuran (0.9M) were introduced. The mixture stood for 20 minutes and 25 ml of ether and 25 ml of water were added. The mixture was extracted with ether and the organic phase was washed with water saturated with sodium chloride, then dried and concentrated to dryness under reduced pressure. The residue was chromatographed over silica and eluted with methylene chloride to obtain 1.44 g of 1,1-dimethylethyl 2-chloro-3-methoxymethyloxirane-carboxylate.

후처리

  1. extractionThe mixture was extracted with ether
  2. washthe organic phase was washed with water saturated with sodium chloride
  3. customdried
  4. concentrationconcentrated to dryness under reduced pressure
  5. customThe residue was chromatographed over silica
  6. washeluted with methylene chloride

출처 및 근거

ORD 기록
ord-b6b0bab6a3454b1386b123a69f0790dd
출처 데이터셋
uspto-grants-1997_11
특허 번호
US05683996

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