Formaldehyde → 2-Cyclohexylprop-2-en-1-al

HRID 634977

反応式

HRID 634977 の反応式
S(=O)(=O)(O)O.C=O.[CH:8]1([CH2:14][CH:15]=[O:16])[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1.[CH2:17](NCC)C>>[CH:8]1([C:14](=[CH2:17])[CH:15]=[O:16])[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1

参加物

5

反応物 4

HCID 712FormaldehydeHCID 1118Sulfuric AcidHCID 8021DiethylamineHCID 3166272-Cyclohexylacetaldehyde

生成物 1

HCID 125770702-Cyclohexylprop-2-en-1-al収率 81%

反応条件

温度
80 °C

実験手順

Successively, sulfuric acid 62% (79.4 g, 0.5 mol), aqueous formaldehyde 35% (82 g, 1.0 mol) and cyclohexyl acetaldehyde (100.8 g, 0.8 mol) were added slowly to diethylamine (73 g, 1.0 mol) at 0° C. After stirring at 80° C. overnight, the reaction mixture was extracted with MTBE. The combined organic phases were washed with H2O until neutral pH was achieved, dried (MgSO4) and concentrated in vacuo. The crude product was distilled under reduced pressure using a Widmer column (10 Torr, 80° C.) yielding 89.5 g (81%) of pure product as colorless oil.

後処理

  1. extractionthe reaction mixture was extracted with MTBE
  2. washThe combined organic phases were washed with H2O until neutral pH
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated in vacuo
  5. distillationThe crude product was distilled under reduced pressure
  6. customa Widmer column (10 Torr, 80° C.)

出典と根拠

ORDレコード
ord-7a4e627e30f7477b81179cf836b5d1b1
出典データセット
uspto-grants-2001_02
特許番号
US06184419B2

関連ノート

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