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Sodium Iodide → HCID 21317577, 화합물

HRID 1833486
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HRID 1833486 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

HCID 21317577HCID 21317577, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-f60af9af56724b8199dca98687a4cdee
출처 데이터셋
uspto-grants-1978_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04066675

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