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

HRID 1460865

반응식

HRID 1460865 반응식
[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]

참가 물질

4

반응물 3

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

생성물 1

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

반응 조건

온도
38 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-78ecc085595b4efea612813bf43074b8
출처 데이터셋
uspto-grants-1991_12
특허 번호
US05072056

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