Potassium Carbonate → 4-(4-Hydroxypiperidin-1-yl)benzaldehyde

HRID 1761818노트

반응식

HRID 1761818 반응식
[OH:1][CH:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.F[C:9]1[CH:16]=[CH:15][C:12]([CH:13]=[O:14])=[CH:11][CH:10]=1.C(=O)([O-])[O-].[K+].[K+]>CS(C)=O>[OH:1][CH:2]1[CH2:7][CH2:6][N:5]([C:9]2[CH:16]=[CH:15][C:12]([CH:13]=[O:14])=[CH:11][CH:10]=2)[CH2:4][CH2:3]1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 680234-FluorobenzaldehydeHCID 79341Piperidin-4-ol

생성물 1

HCID 127174464-(4-Hydroxypiperidin-1-yl)benzaldehyde

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

반응 조건

온도
95 °C

실험 절차

A 2 liter three necked flask fitted with a mechanical stirrer, theromometer and condenser is charged with 180 g of 4-hydroxypiperidine, 74.4 g of 4-fluorobenzaldehyde, 1 ml of Aliquot 336, 750 ml of dimethylsulfoxide and 82.8 g of anhydrous potassium carbonate. The mixture is heated at 95° C. for three days, then the product mixture is cooled and poured into 3 liters of ice water. The resultant solid precipitate is filtered, washed with water, and vacuum dried. The crude product is recrystallized from toluene, m.p. 115°-118° C.

후처리

  1. temperaturethe product mixture is cooled
  2. filtrationThe resultant solid precipitate is filtered
  3. washwashed with water, and vacuum
  4. customdried
  5. customThe crude product is recrystallized from toluene, m.p. 115°-118° C.

출처 및 근거

ORD 기록
ord-91c3f6a03fca4db388c733c79b718e1f
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04828758

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