Diiodomethane → HCID 66738885、化合物

HRID 1888881ノート

反応式

HRID 1888881 の反応式
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]

参加物

5

反応物 3

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

生成物 1

HCID 66738885HCID 66738885、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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 (

出典と根拠

ORDレコード
ord-b9e57d21bf1146769a2662ac0ab2e314
出典データセット
uspto-grants-2013_08
特許番号
US08501940B2

反応ノート

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