Formaldehyde → 2-Nitro-2-phenyl-1,3-propanediol

HRID 1460865

反応式

HRID 1460865 の反応式
[N+:1]([CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)([O-:3])=[O:2].[CH2:11]=[O:12].O.[C:14](=[O:17])([O-])[O-].[Na+].[Na+]>>[N+:1]([C:4]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)([CH2:14][OH:17])[CH2:11][OH:12])([O-:3])=[O:2]

参加物

4

反応物 3

HCID 712FormaldehydeHCID 69321(Nitromethyl)benzeneHCID 2735133Sodium Carbonate Monohydrate

生成物 1

HCID 2243932-Nitro-2-phenyl-1,3-propanediol

反応条件

温度
38 °C

実験手順

100 g. (0.73 mole) of nitromethylbenzene, 131.5 g. (1.61 mole) of 37% formaldehyde and 1.8 g. of sodium carbonate monohydrate are placed in a 500 ml. beaker equipped with a mechanical stirrer. The mixture is stirred, the temperature rises to 38° C. and is maintained at 38° C. by using a cold water bath. After 1 1/2 hours, crystals begin to form. The mixture is diluted with 210 ml. of ice water and stirred at 10° C. for about 2 hours. The mixture is filtered and the filtrate washed with water. The damp cake is placed back in the beaker and 280 ml. of ice water is added. The mixture is stirred for 1 hour, filtered and air dried overnight. The solid is stirred with 250 ml. of toluene for about 1 hour at 10° C. and filtered, then washed with cold toluene and dried. The yield is 112.6 g. of nitrophenyldiol (78%), M.P. 96°-97.5° C.

後処理

  1. custombeaker equipped with a mechanical stirrer
  2. customrises to 38° C.
  3. customAfter 1 1/2 hours, crystals
  4. customto form
  5. additionThe mixture is diluted with 210 ml
  6. filtrationThe mixture is filtered
  7. washthe filtrate washed with water
  8. additionof ice water is added
  9. stirringThe mixture is stirred for 1 hour
  10. filtrationfiltered
  11. customair dried overnight
  12. stirringThe solid is stirred with 250 ml
  13. filtrationfiltered
  14. washwashed with cold toluene
  15. customdried

出典と根拠

ORDレコード
ord-78ecc085595b4efea612813bf43074b8
出典データセット
uspto-grants-1991_12
特許番号
US05072056

関連ノート

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