Isobutyric Acid → 5-Bromo-5-chloro-4-(1,1-dimethoxyethoxy)-2-methyl-6,6,6-trifluorohex-2-ene

HRID 3014

반응식

HRID 3014 반응식
[Br:1][C:2]([Cl:13])([C:9]([F:12])([F:11])[F:10])[CH:3]([OH:8])[CH:4]=[C:5]([CH3:7])[CH3:6].[C:14](OC)([O:18][CH3:19])([O:16][CH3:17])[CH3:15].C(O)(=O)C(C)C>>[Br:1][C:2]([Cl:13])([C:9]([F:10])([F:11])[F:12])[CH:3]([O:8][C:14]([O:18][CH3:19])([O:16][CH3:17])[CH3:15])[CH:4]=[C:5]([CH3:7])[CH3:6]

참가 물질

4

반응물 3

HCID 6590Isobutyric AcidHCID 15050Trimethyl orthoacetateHCID 152193461,1,1-Trifluoro-2-bromo-2-chloro-5-methyl-4-hexen-3-ol

생성물 1

HCID 152787025-Bromo-5-chloro-4-(1,1-dimethoxyethoxy)-2-methyl-6,6,6-trifluorohex-2-ene

반응 조건

온도
111 °C

실험 절차

5-Bromo-5-chloro-4-hydroxy-2-methyl-6,6,6-trifluorohex-2-ene (10.0 g), trimethyl orthoacetate (48.0 g) and isobutyric acid (0.29 g) were charged to a round-bottomed flask fitted with: nitrogen inlet/bubbler, thermometer and Dean and Stark received packed with 5A molecular seives. The mixture was heated with agitation to reflux and distillates collected until reaction mass temperature increased to 111° C. (ca. 1 hr). Once the reaction was complete, the residual trimethyl orthoacetate was removed by distillation under vacuum (ca. 50° C. @ 50 mmHg) to give the product, 5-bromo-5-chloro-4-(1,1-dimethoxyethoxy)-2-methyl-6,6,6-trifluorohex-2-ene, as an orange oil (10.9 g, 85% yield).

후처리

  1. customfitted with: nitrogen inlet/bubbler
  2. temperatureThe mixture was heated with agitation
  3. temperatureto reflux
  4. distillationdistillates collected until reaction mass temperature
  5. customthe residual trimethyl orthoacetate was removed by distillation under vacuum (ca. 50° C. @ 50 mmHg)

출처 및 근거

ORD 기록
ord-5232ccbb96cf4bf19ed922c74f60ad33
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05731475

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