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Isobutyric Acid → HCID 19936152, 화합물

HRID 260611
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HRID 260611 반응식
Br[C:2](Cl)([C:9]([F:12])([F:11])[F:10])[CH:3](O)[CH:4]=[C:5]([CH3:7])[CH3:6].C(OC)(OC)(OC)C.C(O)(=O)C(C)C>>[CH3:6][C:5](=[CH:4][CH2:3][CH2:2][C:9]([F:12])([F:11])[F:10])[CH3:7]
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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 19936152HCID 19936152, 화합물

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온도
111 °C

실험 절차

5-Bromo-5-chloro-4-hydroxy-2-methyl-6,6,6-trifluorohex-2ene (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-fcee9aa287524ea18dc987ee5bcad3e9
출처 데이터셋
uspto-grants-1996_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05527972

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