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

HRID 34123노트

반응식

HRID 34123 반응식
[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]

참가 물질

4

반응물 2

HCID 674DimethylamineHCID 574666101-Methanesulfonyloxymethyl-cyclopropanecarboxylic acid ethyl ester

생성물 1

HCID 60034732Ethyl 1-[(dimethylamino)methyl]cyclopropanecarboxylate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-864b41905396449fbae3ee8dca74fb67
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07429609B2

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