ethyl 3-amino-3-thioxopropanoate → HCID 19790104, 화합물

HRID 1154184노트

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HRID 1154184 반응식
[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]

참가 물질

3

반응물 1

HCID 2771567ethyl 3-amino-3-thioxopropanoate

생성물 1

HCID 19790104HCID 19790104, 화합물수율 106.3%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-d796a0de22de4fa8afebf60371f07306
출처 데이터셋
uspto-grants-1984_12
특허 번호
US04487927

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