Acetic Anhydride → N-(5-nitropyrimidin-2-yl)acetamide

HRID 253698

반응식

HRID 253698 반응식
[NH2:1][C:2]1[N:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][N:3]=1.[C:11](OC(=O)C)(=[O:13])[CH3:12]>C1(C)C=CC=CC=1>[N+:8]([C:5]1[CH:4]=[N:3][C:2]([NH:1][C:11](=[O:13])[CH3:12])=[N:7][CH:6]=1)([O-:10])=[O:9]

참가 물질

4

반응물 2

HCID 7918Acetic Anhydride2회HCID 764905-Nitropyrimidin-2-amine

생성물 1

HCID 45071770N-(5-nitropyrimidin-2-yl)acetamide

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
90 °C

실험 절차

To 2-amino-5-nitropyrimidine (0.42 g, 3.0 mmol) dissolved in toluene (2 ml) was added acetic anhydride (1.4 ml, 15 mmol). The reaction mixture was stirred at 90° C. for 15 hr, after which an additional amount of acetic anhydride was added (0.7 mL) and the mixture was stirred at reflux for another 16 h. The solvent was removed in vacuo and to the residue was added hexane (10 mL) and DCM (1 mL). The solid was collected by filtration, dried to give N-(5-nitropyrimidin-2-yl)acetamide as an off-white solid. MS (ESI, pos. ion) m/z: 183 (M+1).

후처리

  1. stirringthe mixture was stirred
  2. temperatureat reflux for another 16 h
  3. customThe solvent was removed in vacuo and to the residue
  4. additionwas added hexane (10 mL) and DCM (1 mL)
  5. filtrationThe solid was collected by filtration
  6. customdried

출처 및 근거

ORD 기록
ord-e0baeb2ebcfd484482e11216a87fde25
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07872128B2

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