Hydrochloric Acid → HCID 433777, 화합물

HRID 1761938노트

반응식

HRID 1761938 반응식
BrC1C=C[C:5]([O:8]C(F)(F)F)=[CH:4]C=1.[Mg].II.[N:16]1[N:17]([CH:21]([CH3:34])[C:22](C2C=CC(C(F)(F)F)=CC=2)=[O:23])[N:18]=[N:19][CH:20]=1.Cl>O1CCCC1.O>[CH2:5]([O:8][C:22](=[O:23])[CH:21]([N:17]1[N:18]=[N:19][CH:20]=[N:16]1)[CH3:34])[CH3:4]

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 807IodineHCID 5210081-Bromo-4-(trifluoromethoxy)benzeneHCID 5462224MagnesiumHCID 20042602HCID 20042602, 화합물

생성물 1

HCID 433777HCID 433777, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매2회

실험 절차

The Grignard reagent from 4-bromotrifluoromethoxybenzene (2.41 g) was prepared in a similar manner to that described in Example 3 from magnesium turnings (0.24) in dry tetrahydrofuran (14 ml) with iodine (1 crystal) as an activator. To the Grignard solution was added dropwise over 10 minutes 2-(2H-tetrazol-2-yl)p-trifluoromethylpropiophenone from Example 16 (2.7 g in dry tetrahydrofuran (10 ml), then the reaction stirred for 1 hour. The reaction was worked up as for previous examples, by pouring into water, acidifying with aqueous hydrochloric acid and extracting the product into diethyl ether, which was dried over anhydrous sodium sulphate and evaporated. The residual oil (4.3 g) was purified by h.p.l.c. on silica gel eluting with 5:1 hexane/ethyl acetate to give a colourless oil 2.3 g.

후처리

  1. extractionextracting the product into diethyl ether, which
  2. dry with materialwas dried over anhydrous sodium sulphate
  3. customevaporated
  4. customThe residual oil (4.3 g) was purified by h.p.l.c

출처 및 근거

ORD 기록
ord-b10ea6c60d1440499395f9fad1dac228
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04829074

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