4-Hydroxybenzaldehyde → p-Octyloxycarbonyloxybenzaldehyde

HRID 648874

반응식

HRID 648874 반응식
[OH:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=1.Cl[C:11]([O:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])=[O:12].C1(C)C=CC=CC=1.Cl>N1C=CC=CC=1>[CH2:14]([O:13][C:11]([O:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=1)=[O:12])[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21]

참가 물질

6

반응물 4

HCID 1264-HydroxybenzaldehydeHCID 313Hydrochloric AcidHCID 1140TolueneHCID 81956Carbonochloridic acid, octyl ester

생성물 1

HCID 13828007p-Octyloxycarbonyloxybenzaldehyde수율 65.8%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

Commercially available p-hydroxybenzaldehyde (50 g) was dissolved in pyridine (400 ml), followed by dropwise adding octyl chloroformate (85 g) under ice cooling, heating on a water bath, allowing the reaction mixture to stand overnight, adding toluene (300 ml) and 6N hydrochloric acid, separating the liquid layer, further washing with an aqueous solution of 2N NaOH, washing with water, drying and distilling off toluene to obtain a raw product of p-octyloxycarbonyloxybenzaldehyde (75 g).

후처리

  1. temperatureheating on a water bath
  2. customseparating the liquid layer
  3. washfurther washing with an aqueous solution of 2N NaOH
  4. washwashing with water
  5. customdrying
  6. distillationdistilling off toluene

출처 및 근거

ORD 기록
ord-2540e33eaeda41cbb2db7992398f7311
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04737313

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