o-Cyclohexylphenol → 3-Pyridinecarboxylic acid, 2-cyclohexylphenyl ester, hydrochloride

HRID 2059020

반응식

HRID 2059020 반응식
[CH:1]1([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[OH:13])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.Cl.[C:15]([Cl:23])(=[O:22])[C:16]1[CH:21]=[CH:20][CH:19]=[N:18][CH:17]=1>N1C=CC=CC=1>[ClH:23].[C:15]([O:13][C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=1[CH:1]1[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1)(=[O:22])[C:16]1[CH:21]=[CH:20][CH:19]=[N:18][CH:17]=1

참가 물질

4

반응물 2

HCID 8396o-CyclohexylphenolHCID 884383-Pyridinecarbonyl chloride, hydrochloride (1:1)

생성물 1

HCID 30596433-Pyridinecarboxylic acid, 2-cyclohexylphenyl ester, hydrochloride

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
30 °C

실험 절차

15 g (85 mmol) of o-cyclohexylphenol and 16.5 g (93 mmol) of nicotinic acid chloride hydrochloride was mixed with 200 ml of dry pyridine and stirred for 24 hours at 30° C. After cooling precipitated pyridine hydrochloride was sucked off and 300 ml of water added. The precipitated raw product was washed with two 200 ml portions of water, dissolved in alcohol and reduced by means of a rotary evaporator. The remaining viscous oil was dissolved in 500 ml of dry ether and hydrochlorinated with HCl gas. Subsequently, the mixture was filtered, washed with ether and dried.

후처리

  1. temperatureAfter cooling
  2. customprecipitated pyridine hydrochloride
  3. addition300 ml of water added
  4. customThe precipitated raw product
  5. washwas washed with two 200 ml portions of water
  6. dissolutiondissolved in alcohol
  7. customreduced by means of a rotary evaporator
  8. dissolutionThe remaining viscous oil was dissolved in 500 ml of dry ether and hydrochlorinated with HCl gas
  9. filtrationSubsequently, the mixture was filtered
  10. washwashed with ether
  11. customdried

출처 및 근거

ORD 기록
ord-5f004323ff1b4bc3b27c6cb75a6e1e99
출처 데이터셋
uspto-grants-1982_03
특허 번호
US04321268

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