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Chloroform → HCID 53703941、化合物

HRID 1701166
ノート
印刷プレビュー

反応式

HRID 1701166 の反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[CH:13]=[CH:12][C:11]([CH:14]([S:16]([CH2:18][C:19]([OH:21])=[O:20])=[O:17])[CH3:15])=[CH:10][CH:9]=1.[OH-].[K+].[CH:24](Cl)(Cl)Cl.CI>[I-].C([N+](CCCC)(CCCC)CCCC)CCC.O>[CH3:24][O:20][C:19](=[O:21])[CH2:18][S:16]([CH:14]([C:11]1[CH:12]=[CH:13][C:8]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[F:1])=[CH:9][CH:10]=1)[CH3:15])=[O:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6212ChloroformHCID 6328Methyl iodideHCID 14797Potassium HydroxideHCID 20348737HCID 20348737、化合物

生成物 1

HCID 53703941HCID 53703941、化合物

試薬・触媒・溶媒 2

HCID 67553Tetrabutylammonium Iodide触媒
HCID 962
Water
溶媒

実験手順

1.1 gm (3 millimols) of tetrabutylammonium iodide and 3.06 gm (10 millimols) of [1-(2'-fluoro-4-biphenylyl)-ethylsulfinyl]-acetic acid (m.p. 164°-165° C.) were added to a solution of 730 mgm (13 millimols) of potassium hydroxide in 20 ml of water, then 20 ml of chloroform and 2 ml of methyl iodide were added, and the mixture was stirred at room temperature for 10 hours. Afterwards, the organic phase was separated from the neutral aqueous phase, washed with dilute hydrochloric acid and then with water, dried and evaporated. The residue (3.6 gm) was purified by chromatography on 100 gm of silicagel (grain size: 0.05-0.2 mm) with cyclohexane ethyl acetate=1/4. After evaporation of the combined fractions with an Rf -value of 0.4 and recrystallization of the residue from isopropanol, 1.7 gm (53% of theory) of the title compound m.p. 75°-77° C. were obtained.

後処理

  1. customAfterwards, the organic phase was separated from the neutral aqueous phase
  2. washwashed with dilute hydrochloric acid
  3. dry with materialwith water, dried
  4. customevaporated
  5. customThe residue (3.6 gm) was purified by chromatography on 100 gm of silicagel (grain size: 0.05-0.2 mm) with cyclohexane ethyl acetate=1/4
  6. customAfter evaporation of the combined fractions
  7. customwith an Rf -value of 0.4 and recrystallization of the residue from isopropanol, 1.7 gm (53% of theory) of the title compound m.p. 75°-77° C.
  8. customwere obtained

出典と根拠

ORDレコード
ord-5b279a8695ed460f8018d6edb9b30545
出典データセット
uspto-grants-1980_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04191776

反応ノート

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