Acetic Acid → 1,3-Bis(3,5-di-t-butyl-4-hydroxyphenyl)-2-nitropropane

HRID 597700

반응식

HRID 597700 반응식
[OH-].[K+].[N+:3]([CH3:6])([O-:5])=[O:4].[C:7]([C:11]1[CH:16]=[C:15]([CH2:17]OC)[CH:14]=[C:13]([C:20]([CH3:23])([CH3:22])[CH3:21])[C:12]=1[OH:24])([CH3:10])([CH3:9])[CH3:8].[C:25]([OH:28])(=O)[CH3:26]>CO>[C:7]([C:11]1[CH:16]=[C:15]([CH2:17][CH:6]([N+:3]([O-:5])=[O:4])[CH2:17][C:15]2[CH:16]=[C:26]([C:7]([CH3:8])([CH3:9])[CH3:10])[C:25]([OH:28])=[C:13]([C:20]([CH3:23])([CH3:21])[CH3:22])[CH:14]=2)[CH:14]=[C:13]([C:20]([CH3:22])([CH3:21])[CH3:23])[C:12]=1[OH:24])([CH3:9])([CH3:10])[CH3:8]

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 6375NitromethaneHCID 69112,6-Di-tert-butyl-4-(methoxymethyl)phenolHCID 14797Potassium Hydroxide

생성물 1

HCID 214348841,3-Bis(3,5-di-t-butyl-4-hydroxyphenyl)-2-nitropropane

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 14.5 g (0.22 mole) of 85% potassium hydroxide in 300 ml of methanol was added in a stream of nitrogen to exclude air 13.4 g (0.22 mole) of nitromethane and 50.0 g (0.2 mole) of 2,6-di-t-butyl-4-methoxymethylphenol. The magenta solution was stirred for one hour at reflux, with exclusion of air. After cooling somewhat, the solution was neutralized with 13 ml of acetic acid and chilled. A thick paste formed which was filtered, washed and dried. The resulting tan powder (48.1 g, mp 152°-154° C) was recrystallized from 500 ml of heptane, after filtering insoluble matter (10.4 g). The yield of tan crystals was 32.3 g, mp 161°-165° C.

후처리

  1. temperatureat reflux, with exclusion of air
  2. temperatureAfter cooling somewhat
  3. temperaturechilled
  4. customA thick paste formed which
  5. filtrationwas filtered
  6. washwashed
  7. customdried
  8. customThe resulting tan powder (48.1 g, mp 152°-154° C) was recrystallized from 500 ml of heptane
  9. filtrationafter filtering insoluble matter (10.4 g)

출처 및 근거

ORD 기록
ord-62dd71c8cc56468cae5d7144f12ac790
출처 데이터셋
uspto-grants-1977_03
특허 번호
US04014943

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