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

HRID 67072노트

반응식

HRID 67072 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5aa868eed3b24f508e8479e87dceebba
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04344948

반응 노트

불러오는 중…