Magnesium → Methyl 3-cyclopropyl-3-(4-chlorophenyl)propanoate

HRID 1588875노트

반응식

HRID 1588875 반응식
[CH:1]1([C:4]([C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][CH:11]=2)=[CH:5][C:6]([O:8][CH3:9])=[O:7])[CH2:3][CH2:2]1.[Mg]>CO.Cl>[CH:1]1([CH:4]([C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][CH:11]=2)[CH2:5][C:6]([O:8][CH3:9])=[O:7])[CH2:2][CH2:3]1

참가 물질

5

반응물 2

HCID 5462224MagnesiumHCID 53818028Methyl 3-cyclopropyl-3-(4-chlorophenyl)propenoate

생성물 1

HCID 19754833Methyl 3-cyclopropyl-3-(4-chlorophenyl)propanoate수율 62.3%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 887Methanol용매

실험 절차

A mixture of 17.0 grams (0.072 mole) of methyl 3-cyclopropyl-3-(4-chlorophenyl)propenoate and 4.3 grams (0.18 mole) of magnesium in 250 ml of methanol was stirred at ambient temperature for about 3.5 hours. After this time the reaction mixture was carefully diluted with aqueous 3N hydrochloric acid. The mixture was extracted with diethyl ether. The combined ether extracts were dried with sodium sulfate and filtered. The filtrate was concentrated under reduced pressure to a residual oil. The oil was distilled under vacuum, yielding 10.7 grams of methyl 3-cyclopropyl-3-(4-chlorophenyl)propanoate; b.p. 91-97° C./0.10 mm. The spectrum was consistent with the proposed structure.

후처리

  1. extractionThe mixture was extracted with diethyl ether
  2. dry with materialThe combined ether extracts were dried with sodium sulfate
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated under reduced pressure to a residual oil
  5. distillationThe oil was distilled under vacuum

출처 및 근거

ORD 기록
ord-347316cf47e34dd3b75935a93eb9ab0b
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05223536

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