Hydrochloric Acid → HCID 433777、化合物

HRID 1761938ノート

反応式

HRID 1761938 の反応式
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]

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 807IodineHCID 5210081-Bromo-4-(trifluoromethoxy)benzeneHCID 5462224MagnesiumHCID 20042602HCID 20042602、化合物

生成物 1

HCID 433777HCID 433777、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b10ea6c60d1440499395f9fad1dac228
出典データセット
uspto-grants-1989_05
特許番号
US04829074

反応ノート

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