Dimethylformamide dimethyl acetal → 1-Penten-3-one, 1-(dimethylamino)-4,4-dimethoxy-

HRID 1181558노트

반응식

HRID 1181558 반응식
[CH3:1][O:2][C:3]([O:8][CH3:9])([CH3:7])[C:4](=[O:6])[CH3:5].CO[CH:12](OC)[N:13]([CH3:15])[CH3:14]>CO>[CH3:12][N:13]([CH3:15])[CH:14]=[CH:5][C:4](=[O:6])[C:3]([O:8][CH3:9])([O:2][CH3:1])[CH3:7]

참가 물질

4

반응물 2

HCID 78373Dimethylformamide dimethyl acetalHCID 1408713,3-Dimethoxy-2-butanone

생성물 1

HCID 5668111-Penten-3-one, 1-(dimethylamino)-4,4-dimethoxy-수율 90.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

100 g (0.76 mol) of 3,3-dimethoxy-2-butanone (16) were stirred together with 90.2 g of N,N-dimethylformamide dimethyl acetal (17) (0.76 mol) at 120° C. for 48 h. The methanol which was formed in the reaction was removed continuously from the reaction solution by means of distillation. Crystallization occurred spontaneously when the solution was cooled, with the crystallization being brought to completion by adding a little heptane. This resulted in 128.24 g of crude product 18 (yield 90%), which was reacted without any further purification.

후처리

  1. customwas removed continuously from the reaction solution by means of distillation
  2. customCrystallization
  3. temperaturewas cooled, with the crystallization
  4. additionby adding a little heptane

출처 및 근거

ORD 기록
ord-9dce04cd83704e3797829a7b53f6fdaa
출처 데이터셋
uspto-grants-2007_10
특허 번호
US07285560B2

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