Formaldehyde → 3-(Hydroxymethyl)phenytoin

HRID 260209

反応式

HRID 260209 の反応式
[CH:1]1[CH:2]=[CH:3][C:4]([C:7]2([C:14]3[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=3)[NH:12][C:11]([OH:13])=[N:10][C:8]2=[O:9])=[CH:5][CH:6]=1.C=O.[C:22]([O-])([O-])=[O:23].[K+].[K+]>O>[C:14]1([C:7]2([C:4]3[CH:3]=[CH:2][CH:1]=[CH:6][CH:5]=3)[NH:12][C:11](=[O:13])[N:10]([CH2:22][OH:23])[C:8]2=[O:9])[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

参加物

5

反応物 3

HCID 712FormaldehydeHCID 17755,5-DiphenylhydantoinHCID 11430Potassium Carbonate

生成物 1

HCID 1613663-(Hydroxymethyl)phenytoin収率 91%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Phenytoin (5 g, 0.02 mol) was suspended in 180 ml of water; 20 ml of formaldehyde (37% solution) and 0.25 g K2CO3 were added and the mixture was stirred at 25°-30° C. for 24 hours. The white solid which formed was removed by filtration and washed repeatedly with a 3% solution of formaldehyde, then air dried for 3 to 4 hours and over P2O5 in a vacuum dessicator. Yield 91-93%, m.p. 185°-189° C. Anal. calc. for C16H14N2O3 : C, 68.07; H, 5.00; N, 9.93. Found: C, 67.97; H, 5.05; N, 9.93. The product has the formula: ##STR1518##

後処理

  1. customThe white solid which formed
  2. customwas removed by filtration
  3. washwashed repeatedly with a 3% solution of formaldehyde
  4. dry with materialair dried for 3 to 4 hours and over P2O5 in a vacuum dessicator

出典と根拠

ORDレコード
ord-57c0db8ab50541878ca6b647dac2c932
出典データセット
uspto-grants-1996_06
特許番号
US05525727

関連ノート

読み込み中…