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Hydrochloric Acid → 2-(1H-Inden-3-yl)ethyl 4-methylbenzenesulphonate

HRID 260666
ノート
印刷プレビュー

反応式

HRID 260666 の反応式
[CH2:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]([CH2:10][CH2:11][OH:12])=[CH:2]1.[CH3:13][C:14]1[CH:19]=[CH:18][C:17]([S:20](Cl)(=[O:22])=[O:21])=[CH:16][CH:15]=1.Cl>N1C=CC=CC=1>[CH3:13][C:14]1[CH:19]=[CH:18][C:17]([S:20]([O:12][CH2:11][CH2:10][C:3]2[C:4]3[C:9](=[CH:8][CH:7]=[CH:6][CH:5]=3)[CH2:1][CH:2]=2)(=[O:22])=[O:21])=[CH:16][CH:15]=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 313Hydrochloric AcidHCID 73974-Toluenesulfonyl chlorideHCID 113556481H-Indene-3-ethanol

生成物 1

HCID 121780952-(1H-Inden-3-yl)ethyl 4-methylbenzenesulphonate収率 71.8%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

5 g (0.031 mol) of 1H-indene-3-ethanol are dissolved in 50 ml of dry pyridine. The mixture is stirred and cooled using an ice bath, 5.9 g (0.031 mol) of 4-methylbenzenesulphonyl chloride are added in portions, and stirring is continued under cold conditions for 1 h and then at room temperature for 4 h. The solution obtained is poured into a mixture of 100 ml of 10N hydrochloric acid and 200 g of ice. The mixture is extracted twice with diethyl ether, and the organic phase is separated, washed with water, dried over magnesium sulphate and filtered. The filtrate is evaporated under reduced pressure. 7 g of an oily product are obtained which is used as it is in the following step.

後処理

  1. temperaturecooled
  2. stirringstirring
  3. waitat room temperature for 4 h
  4. customThe solution obtained
  5. extractionThe mixture is extracted twice with diethyl ether
  6. customthe organic phase is separated
  7. washwashed with water
  8. dry with materialdried over magnesium sulphate
  9. filtrationfiltered
  10. customThe filtrate is evaporated under reduced pressure

出典と根拠

ORDレコード
ord-88934561421c4dcca73a81f1e7b58d0e
出典データセット
uspto-grants-1996_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05530002

反応ノート

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