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Aluminum isopropoxide → HCID 20163297、化合物

HRID 246893
ノート
印刷プレビュー

反応式

HRID 246893 の反応式
CC([O-])C.CC([O-])C.CC([O-])C.[Al+3].[CH3:14][C:15]1([C:23](=[O:25])[CH3:24])[CH:20]([CH3:21])[CH2:19][C:18]([CH3:22])=[CH:17][CH2:16]1.C(O)(C)C.CC(C)=O>C(O)(C)C>[CH3:14][C:15]1([CH:23]([OH:25])[CH3:24])[CH:20]([CH3:21])[CH2:19][C:18]([CH3:22])=[CH:17][CH2:16]1
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 11143Aluminum isopropoxideHCID 201632901-(1,4,6-Trimethylcyclohex-3-en-1-yl)ethan-1-oneHCID 22386392HCID 22386392、化合物

生成物 1

HCID 20163297HCID 20163297、化合物

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

A solution of 0.33 moles (68 g) aluminum isopropylate in 600 ml isopropanol was heated to boiling in a 1-liter 3-necked flask with a magnetic stirrer, packed column, dropping funnel and thermometer. Within two hours 1 mole (166 g) 1-(1,4,6-trimethylcyclohex-3-en-1-yl)ethan-1-one (as per Example 1) was added dropwise to the boiling solution, and at the same time the isopropanol/acetone mixture formed was distilled off. After 10 hours the reaction was ended (after no more acetone could be detected in the distillate). Thereupon isopropanol still remaining was drawn off, and 175 ml 20% by weight hydrochloric acid was added to the residue after cooling. Extraction was carried out and the organic phase was washed free of acid. After fractional distillation 151 g of the desired end product was obtained, corresponding to 90% of the theoretical amount.

後処理

  1. customto boiling in a 1-liter 3-necked flask with a magnetic stirrer
  2. distillationwas distilled off
  3. addition175 ml 20% by weight hydrochloric acid was added to the residue
  4. temperatureafter cooling
  5. extractionExtraction
  6. washthe organic phase was washed free of acid
  7. distillationAfter fractional distillation 151 g of the desired end product
  8. customwas obtained, corresponding to 90% of the theoretical amount

出典と根拠

ORDレコード
ord-b05917b696c74f1cb3a503a93e53c71c
出典データセット
uspto-grants-1987_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04704477

反応ノート

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