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Sodium Iodide → HCID 21317577、化合物

HRID 1833486
ノート
印刷プレビュー

反応式

HRID 1833486 の反応式
C1(C)C=CC(S(O[CH2:11][CH2:12][CH2:13][CH:14]([O:27][C:28](=[O:30])[CH3:29])[CH2:15][O:16][C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([C:23]([F:26])([F:25])[F:24])[CH:18]=2)(=O)=O)=CC=1.[I-:32].[Na+]>CC(C)=O>[I:32][CH2:11][CH2:12][CH2:13][CH:14]([O:27][C:28](=[O:30])[CH3:29])[CH2:15][O:16][C:17]1[CH:22]=[CH:21][CH:20]=[C:19]([C:23]([F:26])([F:25])[F:24])[CH:18]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 5238Sodium IodideHCID 213176291-(p-Toluenesulfonyloxy)-4-acetoxy-5-(3-trifluoromethylphenoxy)pentane

生成物 1

HCID 21317577HCID 21317577、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A solution of 1-(p-toluenesulfonyloxy)-4-acetoxy-5-(3-trifluoromethylphenoxy)pentane (125 g., 0.28 mole) and sodium iodide (126 g., 0.84 mole) in acetone (600 ml.) is allowed to stand at 25°-27° for 16 hours. The precipitated sodium tosylate is filtered off. Most of the acetone is evaporated from the filtrate and the residue is treated with 300 ml. of water. The oily product is taken up in ether, washed with dilute sodium thiosulfate solution, water, and brine, and dried over magnesium sulfate. The solvent is distilled in vacuo to yield 113 g. (97%) of the crude title compound as a yellowish oil which is used without further purification; pmr (CDCl3) 2.06 (3H, s CH3O); 3.20 (2H, t CH2I); 4.01 (2H, d CH2O); 5.20 (1H, m CHO).

後処理

  1. filtrationThe precipitated sodium tosylate is filtered off
  2. customMost of the acetone is evaporated from the filtrate
  3. additionthe residue is treated with 300 ml
  4. washwashed with dilute sodium thiosulfate solution, water, and brine
  5. dry with materialdried over magnesium sulfate
  6. distillationThe solvent is distilled in vacuo
  7. customto yield 113 g
  8. custom(97%) of the crude title compound as a yellowish oil which is used without further purification

出典と根拠

ORDレコード
ord-f60af9af56724b8199dca98687a4cdee
出典データセット
uspto-grants-1978_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04066675

反応ノート

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