Diiodomethane → HCID 66738885, 화합물

HRID 1888881노트

반응식

HRID 1888881 반응식
C(I)I.[CH2:4]([O:6][C:7](=[O:12])[CH2:8][C:9]([CH3:11])=[CH2:10])[CH3:5].[CH3:13]COC(C)=O>C(OCC)C>[CH2:4]([O:6][C:7](=[O:12])[CH2:8][C:9]1([CH3:13])[CH2:11][CH2:10]1)[CH3:5]

참가 물질

5

반응물 3

HCID 6346DiiodomethaneHCID 8857Ethyl AcetateHCID 30140213-Butenoic acid, 3-methyl-, ethyl ester

생성물 1

HCID 66738885HCID 66738885, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
60 °C

실험 절차

Zn—Cu couple (10.726 g) suspended in diethyl ether (20 ml) was treated at RT under an argon atmosphere with CH2I2 (14.86 g) and 3-methyl-but-3-enoic acid ethyl ester (3.9 g) and heated in a closed reaction vial at 60° C. for 20 h. The mixture was then cooled to RT, AcOEt (50 ml) were added and reaction mixture was filtered. The filter cake was washed with AcOEt, the combined filtrates washed with water (125 ml), dried over MgSO4 and then evaporated (applying a 40 mbar vacuum). This gave the desired (1-methyl-cyclopropyl)-acetic acid ethyl ester (4.4 g) as a brown liquid that was essentially pure (according to NMR) and used directly in the next reaction step.

후처리

  1. temperatureThe mixture was then cooled to RT
  2. customreaction mixture
  3. filtrationwas filtered
  4. washThe filter cake was washed with AcOEt
  5. washthe combined filtrates washed with water (125 ml)
  6. dry with materialdried over MgSO4
  7. customevaporated (

출처 및 근거

ORD 기록
ord-b9e57d21bf1146769a2662ac0ab2e314
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08501940B2

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