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

HRID 868682ノート

反応式

HRID 868682 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 21283660Methyl 3-(3-thienylethyl)aminocrotonate収率 97.5%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

3.8 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-thienyl)ethyl]aminocrotonate intermediate as a slightly yellowish oil.

後処理

  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

出典と根拠

ORDレコード
ord-4686997e6c6b4a52b3007df2e06e64c1
出典データセット
uspto-grants-1988_10
特許番号
US04780538

反応ノート

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