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Hydrochloric Acid → HCID 20144978, 화합물

HRID 648593
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HRID 648593 반응식
[CH3:1][NH:2][C:3]1[S:4][C:5]([C:13]2[CH:18]=[CH:17][N:16]=[CH:15][CH:14]=2)=[C:6]([C:8](OCC)=[O:9])[N:7]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].Cl>O1CCCC1>[CH:8]([C:6]1[N:7]=[C:3]([NH:2][CH3:1])[S:4][C:5]=1[C:13]1[CH:18]=[CH:17][N:16]=[CH:15][CH:14]=1)=[O:9]
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 20145031HCID 20145031, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 20144978HCID 20144978, 화합물수율 37%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of ethyl 2-methylamino-5-(4-pyridyl)-4-thiazolecarboxylate (2.6 g) in dry tetrahydrofuran (120 ml) was added lithium aluminum hydride (0.38 g) at -10° C. with stirring, which was continued at -10°~-3° C. for 30 minutes. The reaction mixture was poured into ice-water and the resultant solution was acidified to pH 1.0 with 10% hydrochloric acid. The insoluble material was filtered off. The filtrate was adjusted to pH 7.0 with 20% aqueous solution of potassium carbonate and extracted with a mixture of ethyl acetate and tetrahydrofuran. The organic extract was concentrated in vacuo. The precipitate was collected by filtration, washed with ethyl acetate and dried in vacuo to give 4-formyl-2-methylamino-5-(4-pyridyl)thiazole (0.8 g). mp 243°-245° C. (dec.).

후처리

  1. filtrationThe insoluble material was filtered off
  2. extractionextracted with a mixture of ethyl acetate and tetrahydrofuran
  3. extractionThe organic extract
  4. concentrationwas concentrated in vacuo
  5. filtrationThe precipitate was collected by filtration
  6. washwashed with ethyl acetate
  7. customdried in vacuo

출처 및 근거

ORD 기록
ord-1bcb5a6bd21546368b021bf63e7ee962
출처 데이터셋
uspto-grants-1988_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04735957

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