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Pyridine → HCID 15729154, 화합물

HRID 1656955
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HRID 1656955 반응식
[NH2:1][C:2]1[S:3][C:4]([S:7][C:8]2[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][CH:9]=2)=[CH:5][N:6]=1.N1C=CC=CC=1.[C:23](Cl)(=[O:26])[CH2:24][CH3:25].C(=O)(O)[O-].[Na+]>CN(C)C=O>[C:23]([NH:1][C:2]1[S:3][C:4]([S:7][C:8]2[CH:9]=[CH:10][C:11]([N+:14]([O-:16])=[O:15])=[CH:12][CH:13]=2)=[CH:5][N:6]=1)(=[O:26])[CH2:24][CH3:25]
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참가 물질

6

반응물 4

HCID 1049PyridineHCID 62324Propionyl chlorideHCID 350381HCID 350381, 화합물HCID 516892Sodium Bicarbonate

생성물 1

HCID 15729154HCID 15729154, 화합물수율 78.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a mixture of 2-amino-5-(4-nitrophenylthio)thiazole (2.6 g) and pyridine (1 g) in N,N-dimethylformamide (30 ml) was added dropwise the propionylchloride (1.1 g) at 5° C. under ice cooling with stirring. The mixture was stirred at 5° C. for 3.5 hours. The reaction mixture was poured into ice water and the mixture was adjusted to pH 8 using aqueous sodium bicarbonate. The precipitates were collected by filtration, washed with water and dried in vacuo to give 2-propionylamino-5-(4-nitrophenylthio)thiazole (2.5 g, yield: 78.7%). mp: 227°-229° C. (dec.)

후처리

  1. stirringThe mixture was stirred at 5° C. for 3.5 hours
  2. filtrationThe precipitates were collected by filtration
  3. washwashed with water
  4. customdried in vacuo

출처 및 근거

ORD 기록
ord-e33e66ca76a34af58ea63d1c43ef753e
출처 데이터셋
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05256675

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