Dimethylamine → Ethyl 1-[(dimethylamino)methyl]cyclopropanecarboxylate

HRID 34123

反応式

HRID 34123 の反応式
[CH2:1]([O:3][C:4]([C:6]1([CH2:9]OS(C)(=O)=O)[CH2:8][CH2:7]1)=[O:5])[CH3:2].[CH3:15][NH:16][CH3:17]>O1CCCC1>[CH2:1]([O:3][C:4]([C:6]1([CH2:9][N:16]([CH3:17])[CH3:15])[CH2:8][CH2:7]1)=[O:5])[CH3:2]

参加物

4

実験手順

To a solution of 222 mg of 1-methanesulfonyloxymethyl-cyclopropane carboxylic acid ethyl ester in 5 mL of tetrahydrofuran was added 3 mL of 2M dimethyl amine in tetrahydrofuran, and stirred at room temperature for 3 days. The solvent was distilled off, and the residue was added with 2 mL of 1N hydrochloric acid, and washed with diethyl ether. The aqueous layer was added with 10% potassium carbonate aqueous solution, and extracted with ethyl acetate. The extracted layer was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated, to afford 56 mg of the title compound as a pale yellow oil.

後処理

  1. distillationThe solvent was distilled off
  2. additionthe residue was added with 2 mL of 1N hydrochloric acid
  3. washwashed with diethyl ether
  4. additionThe aqueous layer was added with 10% potassium carbonate aqueous solution
  5. extractionextracted with ethyl acetate
  6. washThe extracted layer was washed with saturated brine
  7. dry with materialdried over anhydrous magnesium sulfate
  8. customThe solvent was evaporated

出典と根拠

ORDレコード
ord-864b41905396449fbae3ee8dca74fb67
出典データセット
uspto-grants-2008_09
特許番号
US07429609B2

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