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

HRID 253698

反応式

HRID 253698 の反応式
[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]

参加物

4

反応物 2

HCID 7918Acetic Anhydride2 回HCID 764905-Nitropyrimidin-2-amine

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
90 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-e0baeb2ebcfd484482e11216a87fde25
出典データセット
uspto-grants-2011_01
特許番号
US07872128B2

関連ノート

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