Sodium borohydride → 1-[2-(3-Chlorophenyl)-2-hydroxyethyl]-4-[3,4-dihydro-2(1H)-quinazolinon-3-yl]-piperidine

HRID 67079

反応式

HRID 67079 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:25]=[CH:26][CH:27]=1)[C:5]([CH2:7][N:8]1[CH2:13][CH2:12][CH:11]([N:14]2[CH2:23][C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[NH:16][C:15]2=[O:24])[CH2:10][CH2:9]1)=[O:6].[BH4-].[Na+]>CO>[Cl:1][C:2]1[CH:3]=[C:4]([CH:5]([OH:6])[CH2:7][N:8]2[CH2:9][CH2:10][CH:11]([N:14]3[CH2:23][C:22]4[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=4)[NH:16][C:15]3=[O:24])[CH2:12][CH2:13]2)[CH:25]=[CH:26][CH:27]=1

参加物

4

反応物 2

HCID 4311764Sodium borohydrideHCID 127979921-(3-chlorobenzoylmethyl)-4-[3,4-dihydro-2(1H)-quinazolinon-3-yl]-piperidine

生成物 1

HCID 127979951-[2-(3-Chlorophenyl)-2-hydroxyethyl]-4-[3,4-dihydro-2(1H)-quinazolinon-3-yl]-piperidine収率 57.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

In this example, 1.50 g of 1-(3-chlorobenzoylmethyl)-4-[3,4-dihydro-2(1H)-quinazolinon-3-yl]-piperidine and 75 ml of methanol are mixed and stirred at room temperature. To the stirred mixture, 1.0 g of sodium borohydride is added over a period of 5 hours. Then, the mixture is stirred overnight at room temperature. The white crystals deposited are separated by filtration, successively washed with methanol and water and dried to obtain 1.21 g of a crude product. The crude product is recrystallized from a mixed solvent of chloroform and ethanol to obtain 0.87 g of the desired product.

後処理

  1. stirringThen, the mixture is stirred overnight at room temperature
  2. customThe white crystals deposited are separated by filtration
  3. washsuccessively washed with methanol and water
  4. customdried
  5. customto obtain 1.21 g of a crude product
  6. customThe crude product is recrystallized from a mixed solvent of chloroform and ethanol

出典と根拠

ORDレコード
ord-f4516bc0a6da42d782e6c4c4feee987e
出典データセット
uspto-grants-1982_08
特許番号
US04344948

関連ノート

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