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Hydrochloric Acid → 3-Bromo-4-n-butoxy-1,1,1-trifluorobut-3-en-2-one

HRID 2352413
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인쇄 미리보기

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HRID 2352413 반응식
[Br:1]Br.[CH2:3]([O:7][CH:8]=[CH:9][C:10](=[O:15])[C:11]([F:14])([F:13])[F:12])[CH2:4][CH2:5][CH3:6].C(N(CC)CC)C.Cl>CCCCC>[Br:1][C:9](=[CH:8][O:7][CH2:3][CH2:4][CH2:5][CH3:6])[C:10](=[O:15])[C:11]([F:13])([F:14])[F:12]
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 24408BromineHCID 2782641Butoxyvinyl trifluoromethyl ketone

생성물 1

HCID 540224253-Bromo-4-n-butoxy-1,1,1-trifluorobut-3-en-2-one

시약·촉매·용매 1

HCID 8003Pentane용매3회

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온도
-20 °C

실험 절차

8.0 g (0.05 mole) of bromine, dissolved in 100 ml pentane, are added dropwise to a solution of 9.75 g (0.05 mol) of 4-n-butoxy-1,1,1-trifluorobut-3-en-2-one in 50 ml of pentane cooled to -20° C. After stirring for 1 hour at -20° C., a solution of 6.0 g (0.06 mole) of triethylamine in 100 ml pentane is added dropwise at the same temperature. After being allowed to stand overnight at 25° C., the mixture is poured into ice water and acidified by means of 1N hydrochloric acid and the phases are separated. Conventional work-up gives 12.1 g of almost homogeneous crude 3-bromo-4-n-butoxy-1,1,1-trifluorobut-3-en-2-one, which is freed from the small amount of impurities by distillation under reduced pressure. Boiling point 113°-115° C./16 mbar, nD20 =1.4640.

후처리

  1. waitto stand overnight at 25° C.
  2. customthe phases are separated

출처 및 근거

ORD 기록
ord-c4781c4695bd4daa887c88383a984d49
출처 데이터셋
uspto-grants-1989_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04876393

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