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Hexane → HCID 19744803、化合物

HRID 2254401
ノート
印刷プレビュー

反応式

HRID 2254401 の反応式
[CH2:1]([S:8][C:9]1[CH:10]=[C:11]([CH:14]=[CH:15][CH:16]=1)[CH2:12]O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.S(Cl)([Cl:19])=O.CCCCCC>C(Cl)(Cl)Cl>[CH2:1]([S:8][C:9]1[CH:10]=[C:11]([CH:14]=[CH:15][CH:16]=1)[CH2:12][Cl:19])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8058HexaneHCID 24386Thionyl ChlorideHCID 537539293-[(Phenylmethyl)thio]benzenemethanol

生成物 1

HCID 19744803HCID 19744803、化合物収率 51%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

One hundred milligrams of the alcohol obtained above was dissolved in 10 ml of chloroform, and 0.3 ml of thionyl chloride was added. The mixture was reacted at room temperature for 2 hours. The reaction mixture was concentrated under reduced pressure, and the residue was dissolved in 20 ml of water and 20 ml of ethyl ether. The ether layer was separated, and the solvent was evaporated. The residue was purified by medium-pressure liquid chromatography column: Lobar column, size A, Lichroprep Si 60F (a product of E. Merck Co.); eluting solvent: hexane] to give 55 mg (yield 51%) of 3-benzylthiobenzyl chloride as a colorless oil.

後処理

  1. customThe mixture was reacted at room temperature for 2 hours
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. dissolutionthe residue was dissolved in 20 ml of water
  4. customThe ether layer was separated
  5. customthe solvent was evaporated
  6. customThe residue was purified by medium-pressure liquid chromatography column

出典と根拠

ORDレコード
ord-e0f6b05258e447b39b0a545cf2d3f727
出典データセット
uspto-grants-1993_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05234946

反応ノート

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