4-Piperidineethanol → HCID 13336380、化合物

HRID 986288ノート

反応式

HRID 986288 の反応式
[C:1]1([C:7]2[N:16]=[C:15]([C:17]([O:19]CC)=O)[C:14]3[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=3)[N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[NH:22]1[CH2:27][CH2:26][CH:25]([CH2:28][CH2:29][OH:30])[CH2:24][CH2:23]1>O>[C:1]1([C:7]2[N:16]=[C:15]([C:17]([N:22]3[CH2:27][CH2:26][CH:25]([CH2:28][CH2:29][OH:30])[CH2:24][CH2:23]3)=[O:19])[C:14]3[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=3)[N:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

4

反応物 2

HCID 739534-PiperidineethanolHCID 20158356HCID 20158356、化合物

生成物 1

HCID 13336380HCID 13336380、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Ethyl 2-phenylquinazoline-4-carboxylate (1.7 g) and piperidine-4-ethanol (8 g) are heated at 150° C. for 4 hours. After cooling, water is added and the mixture is extracted with ethyl acetate. The organic phase is dried over magnesium sulphate and evaporated to dryness under reduced pressure. The residue is chromatographed on silica gel with ethyl acetate as the eluant, and the product recovered is recrystallized from isopropyl ether. This gives 1-[(2-phenylquinazolin-4-yl)-carbonyl]-piperidine-4-ethanol (0.5 g), melting at 146° C.

後処理

  1. temperatureAfter cooling
  2. extractionthe mixture is extracted with ethyl acetate
  3. dry with materialThe organic phase is dried over magnesium sulphate
  4. customevaporated to dryness under reduced pressure
  5. customThe residue is chromatographed on silica gel with ethyl acetate as the eluant
  6. customthe product recovered
  7. customis recrystallized from isopropyl ether

出典と根拠

ORDレコード
ord-670b5c065a944f6995ddfc6a0c7e14ac
出典データセット
uspto-grants-1987_12
特許番号
US04711890

反応ノート

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