2,2,4-Trimethyl-1,3-pentanediol → 3-Hydroxy-2,2,4-trimethylpentyl 2,2,4-trimethyl-3-oxopentanoate

HRID 572711

反応式

HRID 572711 の反応式
[CH3:1][C:2]1([CH3:10])[C:5](=[O:6])[C:4]([CH3:8])([CH3:7])[C:3]1=[O:9].[CH3:11][CH:12]([CH:14]([OH:20])[C:15]([CH2:18][OH:19])([CH3:17])[CH3:16])[CH3:13].C(=O)([O-])[O-].[K+].[K+]>C1(C)C=CC=CC=1>[CH3:7][C:4]([CH3:8])([C:5](=[O:6])[CH:2]([CH3:10])[CH3:1])[C:3]([O:19][CH2:18][C:15]([CH3:17])([CH3:16])[CH:14]([OH:20])[CH:12]([CH3:13])[CH3:11])=[O:9]

参加物

5

反応物 3

HCID 89462,2,4-Trimethyl-1,3-pentanediolHCID 11430Potassium CarbonateHCID 136172,2,4,4-Tetramethyl-1,3-cyclobutanedione

生成物 1

HCID 885366713-Hydroxy-2,2,4-trimethylpentyl 2,2,4-trimethyl-3-oxopentanoate収率 96%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
120 °C

実験手順

To a 1-liter round bottom flask was charged 2,2,4,4-tetramethyl-1,3-cyclobutanedione (140.2 g, 1.0 moles), TMPD glycol (146.2 g, 1.0 moles) and potassium carbonate (73 g, 0.53 moles). The mixture was heated to 120° C. and held for 4 hours. Reaction was cooled and 200 mL of toluene added. Organic layer was washed 4 times at 70° C. Toluene removed to provide 275 g of product. GC assay of the product was 95.9% (4.6:1 mixture of two major isomers).

後処理

  1. customReaction
  2. temperaturewas cooled
  3. washOrganic layer was washed 4 times at 70° C
  4. customToluene removed

出典と根拠

ORDレコード
ord-f87d7ae9aaa0481cb8a4d9ee5db5f77a
出典データセット
uspto-grants-2015_05
特許番号
US09029451B2

関連ノート

読み込み中…