Tert-butyl ethyl (5-nitropyrazin-2-yl)propanedioate → Ethyl 2-(5-nitropyrazin-2-yl)acetate

HRID 2173328ノート

反応式

HRID 2173328 の反応式
[N+:1]([C:4]1[N:5]=[CH:6][C:7]([CH:10](C(OCC)=O)[C:11]([O:13][C:14](C)(C)[CH3:15])=[O:12])=[N:8][CH:9]=1)([O-:3])=[O:2]>C(O)(C(F)(F)F)=O.C(Cl)Cl>[N+:1]([C:4]1[N:5]=[CH:6][C:7]([CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])=[N:8][CH:9]=1)([O-:3])=[O:2]

参加物

4

反応物 1

HCID 86693017Tert-butyl ethyl (5-nitropyrazin-2-yl)propanedioate

生成物 1

HCID 77230650Ethyl 2-(5-nitropyrazin-2-yl)acetate

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 6422Trifluoroacetic acid溶媒

反応条件

温度
35 °C

実験手順

A mixture of tert-butyl ethyl (5-nitropyrazin-2-yl)propanedioate (10.7 g, 34.4 mmol) in 30 mL of TFA and 30 mL DCM was stirred at 35° C. for 3 hours before concentrated to dryness. The residue was dissolved in 200 mL of EtOAc and washed with water (25 mL) and brine (25 mL), dried over anhydrous Na2SO4 and concentrated to afford ethyl (5-nitropyrazin-2-yl)acetate.

後処理

  1. concentrationbefore concentrated to dryness
  2. dissolutionThe residue was dissolved in 200 mL of EtOAc
  3. washwashed with water (25 mL) and brine (25 mL)
  4. dry with materialdried over anhydrous Na2SO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-3e5d3563466f481f81fe9520e2bfde19
出典データセット
uspto-grants-2015_06
特許番号
US09056859B2

反応ノート

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