Dimethylformamide dimethyl acetal → 3-(Dimethylaminomethyleneamino)benzofuran-2-carboxylic Acid Ethyl Ester

HRID 989329

反応式

HRID 989329 の反応式
[NH2:1][C:2]1[C:3]2[CH:15]=[CH:14][CH:13]=[CH:12][C:4]=2[O:5][C:6]=1[C:7]([O:9][CH2:10][CH3:11])=[O:8].CO[CH:18](OC)[N:19]([CH3:21])[CH3:20]>>[CH2:10]([O:9][C:7]([C:6]1[O:5][C:4]2[CH:12]=[CH:13][CH:14]=[CH:15][C:3]=2[C:2]=1[N:1]=[CH:18][N:19]([CH3:21])[CH3:20])=[O:8])[CH3:11]

参加物

3

反応物 2

HCID 78373Dimethylformamide dimethyl acetalHCID 2063537Ethyl 3-aminobenzofuran-2-carboxylate

生成物 1

HCID 98349623-(Dimethylaminomethyleneamino)benzofuran-2-carboxylic Acid Ethyl Ester収率 75%

実験手順

A mixture of 4.2 g (20.0 mmol) of ethyl 3-amino -2-benzo[b]furancarboxylate (EP 187487 A1) in 10 mL of N,N-dimethylformamide dimethyl acetal is heated at reflux temperature for 1.5 hours, then cooled to room temperature and concentrated in vacuo. The residue is partitioned between ethyl acetate and water. The organic layer is washed with water, dried over sodium sulfate, passed through a pad of diatomaceous earth and concentrated in vacuo. The solid is collected by filtration to provide 3.90 g (75%) of a white solid, mp 89-90° C.

後処理

  1. temperatureis heated
  2. temperatureat reflux temperature for 1.5 hours
  3. concentrationconcentrated in vacuo
  4. customThe residue is partitioned between ethyl acetate and water
  5. washThe organic layer is washed with water
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated in vacuo
  8. filtrationThe solid is collected by filtration

出典と根拠

ORDレコード
ord-716633f7c88a4e42816b7fa46de0818f
出典データセット
uspto-grants-2003_10
特許番号
US06638929B2

関連ノート

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