Tetrahydrofuran → Formic acid (2-formylamino-5-methoxybenzyl)ester

HRID 350608

反応式

HRID 350608 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[CH2:10][OH:11].C([CH2:14][O:15]C=O)#N.[O:18]1CCC[CH2:19]1>>[CH:14]([NH:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[CH2:10][O:11][CH:19]=[O:18])=[O:15]

参加物

4

反応物 3

HCID 8028TetrahydrofuranHCID 4205685(Formyloxy)acetonitrileHCID 13756678(2-Amino-5-methoxyphenyl)methanol

生成物 1

HCID 86596179Formic acid (2-formylamino-5-methoxybenzyl)ester

反応条件

温度
0 °C

実験手順

A solution of 7.00 g of (2-amino-5-methoxyphenyl)methanol, 9.8 ml of formic acid cyanomethyl ester and 0.05 g of 4-N,N-(dimethylamino)pyridine in 30 ml of anhydrous tetrahydrofuran was heated for 5 hours under reflux. The solution was then concentrated by evaporation in vacuo and the residue was taken up in 100 ml of ethyl acetate. Crystals formed on cooling the solution to 0° C., which were suction filtered, washed with methanol, and dried in vacuo. 7.20 g (75% of theory) of the title compound were thereby obtained.

後処理

  1. temperatureunder reflux
  2. concentrationThe solution was then concentrated by evaporation in vacuo
  3. customCrystals formed
  4. filtrationfiltered
  5. washwashed with methanol
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-277ff5e3f8794036a77bcf51628f651d
出典データセット
uspto-grants-2007_02
特許番号
US07183274B2

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