Hydrochloric Acid → 78016-72-5

HRID 500292ノート

反応式

HRID 500292 の反応式
[C:1]1([CH3:11])[CH:6]=[CH:5][C:4]([S:7](Cl)(=[O:9])=[O:8])=[CH:3][CH:2]=1.[CH2:12]([CH:14]([CH2:17][CH2:18][CH2:19][CH3:20])[CH2:15][OH:16])[CH3:13].Cl>N1C=CC=CC=1>[C:1]1([CH3:11])[CH:6]=[CH:5][C:4]([S:7]([O:16][CH2:15][CH:14]([CH2:12][CH3:13])[CH2:17][CH2:18][CH2:19][CH3:20])(=[O:9])=[O:8])=[CH:3][CH:2]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 73974-Toluenesulfonyl chlorideHCID 77202-Ethylhexanol

生成物 1

HCID 1281542778016-72-5収率 87.5%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
0 °C

実験手順

In a 1-L round-bottomed flask containing 250 mL of pyridine, added was 75 g of p-toluenesulfonyl chloride. After the reaction solution was cooled to 0° C., 34 g of 2-ethylhexanol was added dropwise over 30 minutes, and the resulting mixture was left at 0° C. while cooled overnight. The reaction solution was poured into cold 1N hydrochloric acid; the product was extracted with ethyl acetate; and the organic layer was washed with 1N hydrochloric acid until the aqueous hydrochloric acid layer became acidic. The organic layer was dried over magnesium sulfate and evaporated, to give 65 g of 2-ethylhexyl p-toluenesulfonate. The fact that the product is the desirable compound was confirmed with NMR, IR, and mass spectrometry spectra.

後処理

  1. additionadded
  2. waitthe resulting mixture was left at 0° C.
  3. temperaturewhile cooled overnight
  4. extractionthe product was extracted with ethyl acetate
  5. washand the organic layer was washed with 1N hydrochloric acid until the aqueous hydrochloric acid layer
  6. dry with materialThe organic layer was dried over magnesium sulfate
  7. customevaporated

出典と根拠

ORDレコード
ord-fc56640a133b487789a12c25e76890a0
出典データセット
uspto-grants-2010_08
特許番号
US07771916B2

反応ノート

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