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

HRID 597700

反応式

HRID 597700 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-62dd71c8cc56468cae5d7144f12ac790
出典データセット
uspto-grants-1977_03
特許番号
US04014943

関連ノート

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