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Triethylamine → 4-Methyl-4-(3,5-di-tert-butyl-4-hydroxyphenylthio)-2-pentanone

HRID 65167
ノート
印刷プレビュー

反応式

HRID 65167 の反応式
[O:1]=[C:2]([CH:4]=[C:5]([CH3:7])[CH3:6])[CH3:3].[C:8]([C:12]1[CH:17]=[C:16]([SH:18])[CH:15]=[C:14]([C:19]([CH3:22])([CH3:21])[CH3:20])[C:13]=1[OH:23])([CH3:11])([CH3:10])[CH3:9].C(N(CC)CC)C>C1(C)C=CC=CC=1>[CH3:6][C:5]([S:18][C:16]1[CH:15]=[C:14]([C:19]([CH3:20])([CH3:21])[CH3:22])[C:13]([OH:23])=[C:12]([C:8]([CH3:11])([CH3:10])[CH3:9])[CH:17]=1)([CH3:7])[CH2:4][C:2](=[O:1])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 8858Mesityl oxideHCID 703702,6-Di-tert-butyl-4-mercaptophenol

生成物 1

HCID 136435724-Methyl-4-(3,5-di-tert-butyl-4-hydroxyphenylthio)-2-pentanone

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

8.48 Grams of mesityl oxide (0.084 moles) is added dropwise to a solution of 21.0 grams of 2,6 di-tert-butyl-4-mercaptophenol (0.088 moles) and one gram of triethylamine in 30 ml of toluene. The mixture is heated at 50°-55° C. for six hours. The solvent is then stripped off under vacuum and the residue retained at 60°-65° C. and 0.20 mm. Hg. for two hours. The residue is dissolved in toluene and purified by flash chromatography using silica gel. The product is isolated from solution by distilling off the volatiles under vacuum to a final pressure of 0.10 mm. Hg for five hours.

後処理

  1. temperatureThe mixture is heated at 50°-55° C. for six hours
  2. customretained at 60°-65° C.
  3. custompurified by flash chromatography
  4. customThe product is isolated from solution
  5. distillationby distilling off the volatiles under vacuum to a final pressure of 0.10 mm. Hg for five hours

出典と根拠

ORDレコード
ord-d4de8aeca9ca45eda5bfc5d0c2ea9d50
出典データセット
uspto-grants-1986_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04612341

反応ノート

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