Dimethylformamide → Methyl 4-dimethylaminovinyl-3-nitrobenzoate

HRID 853718

反応式

HRID 853718 の反応式
[CH3:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13].CO[CH:17](OC)[N:18]([CH3:20])[CH3:19].CN(C)C=O>CO>[CH3:17][N:18]([CH:20]=[CH:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13])[CH3:19]

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 78373Dimethylformamide dimethyl acetalHCID 81816Methyl 4-methyl-3-nitrobenzoate

生成物 1

HCID 894336Methyl 4-dimethylaminovinyl-3-nitrobenzoate収率 91.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
120 °C

実験手順

Into a reaction flask were introduced 89.7 g of methyl 4-methyl-3-nitrobenzoate, 82.1 g of dimethylformamide dimethyl acetal and 200 ml of dimethylformamide (DMF), and the content of the flask was stirred at 120° C. for 6 hours. DMF was distilled off to obtain a red-violet colored solid product. Then, 300 ml of methanol was poured into the flask to wash the crystalline matter, and filtered. Thus, 104.8 g (yield 91%) of methyl 4-dimethylaminovinyl-3-nitrobenzoate was obtained.

後処理

  1. distillationDMF was distilled off
  2. customto obtain a red-violet colored solid product
  3. washto wash the crystalline matter
  4. filtrationfiltered

出典と根拠

ORDレコード
ord-dd183e029041473db1d15207a584b189
出典データセット
uspto-grants-2007_08
特許番号
US07255779B2

関連ノート

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