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

HRID 634977

반응식

HRID 634977 반응식
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

참가 물질

5

반응물 4

HCID 712FormaldehydeHCID 1118Sulfuric AcidHCID 8021DiethylamineHCID 3166272-Cyclohexylacetaldehyde

생성물 1

HCID 125770702-Cyclohexylprop-2-en-1-al수율 81%

반응 조건

온도
80 °C

실험 절차

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.

후처리

  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.)

출처 및 근거

ORD 기록
ord-7a4e627e30f7477b81179cf836b5d1b1
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06184419B2

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