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

HRID 2072610ノート

反応式

HRID 2072610 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
95 °C

実験手順

A 2 liter three necked flask fitted with a mechanical stirrer, thermometer 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.

後処理

  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.

出典と根拠

ORDレコード
ord-2cea1c96852a4c4eba3a53f38de704a0
出典データセット
uspto-grants-1990_04
特許番号
US04913845

反応ノート

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