4-Hydroxybenzaldehyde → p-Octyloxycarbonyloxybenzaldehyde

HRID 1905599

반응식

HRID 1905599 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 to stand overnight, adding toluene (300 ml), further adding 6N-hydrochloric acid, separating the liquid layer, further washing with 2N-NaOH aqueous solution, 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 2N-NaOH aqueous solution
  4. washwashing with water
  5. customdrying
  6. distillationdistilling off toluene

출처 및 근거

ORD 기록
ord-9680c9fed5314658aeb7f9a78be33508
출처 데이터셋
uspto-grants-1987_03
특허 번호
US04647398

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