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

HRID 350608

반응식

HRID 350608 반응식
[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]

참가 물질

4

반응물 3

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

생성물 1

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

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-277ff5e3f8794036a77bcf51628f651d
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07183274B2

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