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Sodium Bicarbonate → Ethyl 2-(2-amino-4-thiazolyl)-2-ethoxyiminoacetate

HRID 364455
노트
인쇄 미리보기

반응식

HRID 364455 반응식
[CH2:1]([O:3][N:4]=[C:5]([C:11](=O)[CH2:12]Cl)[C:6]([O:8][CH2:9][CH3:10])=[O:7])[CH3:2].[NH2:15][C:16]([NH2:18])=[S:17].C([O-])(=O)C.[Na+].C(=O)(O)[O-].[Na+]>O.CO>[NH2:18][C:16]1[S:17][CH:12]=[C:11]([C:5](=[N:4][O:3][CH2:1][CH3:2])[C:6]([O:8][CH2:9][CH3:10])=[O:7])[N:15]=1
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참가 물질

7

반응물 4

HCID 516892Sodium BicarbonateHCID 517045Sodium AcetateHCID 2723790ThioureaHCID 53877278Ethyl 4-chloro-2-(ethoxyimino)-3-oxobutanoate

생성물 1

HCID 53897917Ethyl 2-(2-amino-4-thiazolyl)-2-ethoxyiminoacetate수율 34.8%

시약·촉매·용매 2

HCID 887Methanol
용매
HCID 962Water용매

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온도
48 °C

실험 절차

A mixture of ethyl 2-ethoxyimino-3-oxo-4-chlorobutyrate (syn isomer 38.7 g.), thiourea (13.2 g.), sodium acetate (14.3 g.), methanol (95 ml.) and water (95 ml.) was stirred at 48° C. for 40 minutes. After the resultant solution was adjusted to pH 6.5 with an aqueous solution of sodium bicarbonate, the appeared precipitates were collected by filtration and washed with diisopropyl ether to give ethyl 2-(2-amino-4-thiazolyl)-2-ethoxyiminoacetate (syn isomer, 14.7 g.), mp 130° to 131° C.

후처리

  1. customthe appeared precipitates
  2. filtrationwere collected by filtration
  3. washwashed with diisopropyl ether

출처 및 근거

ORD 기록
ord-329e70042fb745ca8ddc1352ad3e04eb
출처 데이터셋
uspto-grants-1986_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04604456

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