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

HRID 67072ノート

反応式

HRID 67072 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:26]=[CH:27][C:28]=1[O:29][CH3:30])[C:6]([CH2:8][N:9]1[CH2:14][CH2:13][CH:12]([N:15]2[CH2:24][C:23]3[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=3)[NH:17][C:16]2=[O:25])[CH2:11][CH2:10]1)=[O:7].[BH4-].[Na+]>CO>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:6]([OH:7])[CH2:8][N:9]2[CH2:10][CH2:11][CH:12]([N:15]3[CH2:24][C:23]4[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=4)[NH:17][C:16]3=[O:25])[CH2:13][CH2:14]2)[CH:26]=[CH:27][C:28]=1[O:29][CH3:30]

参加物

4

反応物 2

HCID 4311764Sodium borohydrideHCID 127979841-(3,4-dimethoxybenzoylmethyl)-4-[3,4-dihydro-2(1H)-quinazolinon-3-yl]-piperidine

生成物 1

HCID 127979861-[2-(3,4-Dimethoxyphenyl)-2-hydroxyethyl]-4-[3,4-dihydro-2(1H)-quinazolinon-3-yl]-piperidine収率 66.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

In this example 2.80 g of 1-(3,4-dimethoxybenzoylmethyl)-4-[3,4-dihydro-2(1H)-quinazolinon-3-yl]-piperidine and 150 ml of methanol are mixed and stirred at room temperature. Then, 460 mg of sodium borohydride is added to the stirred mixture over a period of 30 minutes. Thereafter, 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 2.02 g of a crude product. The crude product is crystallized from hot ethanol to obtain 1.86 g of the desired product.

後処理

  1. stirringThereafter, 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 2.02 g of a crude product
  6. customThe crude product is crystallized from hot ethanol

出典と根拠

ORDレコード
ord-5aa868eed3b24f508e8479e87dceebba
出典データセット
uspto-grants-1982_08
特許番号
US04344948

反応ノート

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