ethyl 3-amino-3-thioxopropanoate → HCID 19790104、化合物

HRID 647691ノート

反応式

HRID 647691 の反応式
[NH2:1][C:2](=[S:9])[CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5]>C(OCC)C>[C:4]([C:3]1[N:1]=[C:2]([CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5])[S:9][CH:2]=1)([OH:6])=[O:5]

参加物

3

反応物 1

HCID 2771567ethyl 3-amino-3-thioxopropanoate

生成物 1

HCID 19790104HCID 19790104、化合物収率 106.3%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

A solution of ethyl 3-amino-3-thioxopropionate (73.5 g) in diethyl ether (100 ml) was added to a solution of bromopiruvic acid (88.5 g) in diethyl ether (300 ml) and stirred for 15 hours at ambient temperature. The precipitates were collected by filtration and added to a mixture of water (500 ml) and diethyl ether (300 ml) and then adjusted to pH 7.5 with 20% aqueous sodium carbonate. The separated aqueous solution was adjusted to pH 1.0 with conc. hydrochloric acid and extracted with diethyl ether. The diethyl ether layer was dried over magnesium sulfate and evaporated. The residue was washed with diisopropyl ether to give ethyl 2-(4-carboxythiazol-2-yl)acetate (57.1 g).

後処理

  1. filtrationThe precipitates were collected by filtration
  2. additionadded to a mixture of water (500 ml) and diethyl ether (300 ml)
  3. extractionextracted with diethyl ether
  4. dry with materialThe diethyl ether layer was dried over magnesium sulfate
  5. customevaporated
  6. washThe residue was washed with diisopropyl ether

出典と根拠

ORDレコード
ord-ebc1091bdaf8444782d83f853c62a12b
出典データセット
uspto-grants-1983_10
特許番号
US04409214

反応ノート

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