Ethyl bromopyruvate → 4-Methyl-2-nitro-phenyl-thiazole-4-carboxylic acid ethyl ester

HRID 227236노트

반응식

HRID 227236 반응식
[CH3:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([NH2:8])=[S:7])=[C:4]([N+:11]([O-:13])=[O:12])[CH:3]=1.[CH3:14][CH2:15][O:16][C:17]([C:19]([CH2:21]Br)=O)=[O:18]>CCO.CCOC(C)=O>[CH2:15]([O:16][C:17]([C:19]1[N:8]=[C:6]([C:5]2[CH:9]=[CH:10][C:2]([CH3:1])=[CH:3][C:4]=2[N+:11]([O-:13])=[O:12])[S:7][CH:21]=1)=[O:18])[CH3:14]

참가 물질

5

반응물 2

HCID 66144Ethyl bromopyruvateHCID 541688084-Methyl-2-nitro-thiobenzamide

생성물 1

HCID 866229124-Methyl-2-nitro-phenyl-thiazole-4-carboxylic acid ethyl ester

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8857Ethyl Acetate용매

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온도
70 °C

실험 절차

4-Methyl-2-nitro-thio benzamide (60 mgs, 0.30 mmol, prepared as described in compound 5, Step 2, was stirred in 1 mL absolute EtOH at room temperature under N2. Ethyl bromo pyruvate (65 mgs, 0.33 mmol) was added, and the resulting solution was heated to 70° C. for 3 h. The reaction was diluted to 30 mL with EtOAc and washed with saturated NaHCO3, and saturated NaCl. The organic layer was dried over MgSO4, filtered and concentrated to a yellow oil, which was used as is in the next step.

후처리

  1. washwashed with saturated NaHCO3, and saturated NaCl
  2. dry with materialThe organic layer was dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated to a yellow oil, which

출처 및 근거

ORD 기록
ord-0071cf80c814424a9604bf2d5f427a1a
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07560462B2

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