Methyl acetoacetate → Methyl 3-(3-thienylethyl)aminocrotonate

HRID 2232322노트

반응식

HRID 2232322 반응식
[NH2:1][CH2:2][CH2:3][C:4]1[CH:8]=[CH:7][S:6][CH:5]=1.[C:9]([O:15][CH3:16])(=[O:14])[CH2:10][C:11]([CH3:13])=O>C(OCC)C>[S:6]1[CH:7]=[CH:8][C:4]([CH2:3][CH2:2][NH:1]/[C:11](/[CH3:13])=[CH:10]\[C:9]([O:15][CH3:16])=[O:14])=[CH:5]1

참가 물질

4

반응물 2

HCID 7757Methyl acetoacetateHCID 122587372-(3-Thienyl)ethanamine

생성물 1

HCID 21283660Methyl 3-(3-thienylethyl)aminocrotonate수율 97.5%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

3.82 grams (30 millimoles) of 3-(2-aminoethyl)thiophene was added dropwise with stirring at room temperature to 3.6 grams (31 millimoles) of methyl acetoacetate and the stirring was continued over the weekend at ambient temperature. Thereafter, the mixture was diluted with 250 milliliters of diethyl ether and the resulting ether solution washed with 50 milliliters of brine and then dried over sodium sulfate. The ether solvent was then vaporized from the dried and filtered solution to obtain 6.59 grams of a methyl 3-(3-thienylethyl)aminocrotonate intermediate as a slightly yellowish oil.

후처리

  1. customwas continued over the weekend at ambient temperature
  2. washthe resulting ether solution washed with 50 milliliters of brine
  3. dry with materialdried over sodium sulfate
  4. customdried
  5. filtrationfiltered solution

출처 및 근거

ORD 기록
ord-b04af50007da4d988e57016be9bdae39
출처 데이터셋
uspto-grants-1988_11
특허 번호
US04788203

반응 노트

불러오는 중…