Water → 6-(4-Chlorobenzoyl)-3-propargyl-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine-2,4-dione

HRID 1500610노트

반응식

HRID 1500610 반응식
Cl.[CH2:2]([N:5]1[C:10](=[O:11])[C:9]2[CH2:12][NH:13][CH2:14][CH2:15][C:8]=2[NH:7][C:6]1=[O:16])[C:3]#[CH:4].C(N(CC)CC)C.[Cl:24][C:25]1[CH:33]=[CH:32][C:28]([C:29](Cl)=[O:30])=[CH:27][CH:26]=1.O>C(Cl)Cl>[Cl:24][C:25]1[CH:33]=[CH:32][C:28]([C:29]([N:13]2[CH2:14][CH2:15][C:8]3[NH:7][C:6](=[O:16])[N:5]([CH2:2][C:3]#[CH:4])[C:10](=[O:11])[C:9]=3[CH2:12]2)=[O:30])=[CH:27][CH:26]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 85014-Chlorobenzoyl chlorideHCID 866631133-Propargyl-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine-2,4-dione hydrochloride

생성물 1

HCID 866631156-(4-Chlorobenzoyl)-3-propargyl-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine-2,4-dione

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

3-propargyl-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine-2,4-dione hydrochloride (790 mg) was suspended in methylene chloride, triethylamine (0.95 ml) and 4-chlorobenzoyl chloride (0.42 ml) were added under ice cooling and the resultant mixture was stirred at the same temperature for 30 minutes. To the reaction solution, water was added and the resultant mixture was concentrated. To the residue, diethyl ether was added and insoluble matter was separated by filtration to obtain the titled compound (894 mg) as a white powder. The resultant compound was used in a next reaction without further purifying.

후처리

  1. concentrationthe resultant mixture was concentrated
  2. additionTo the residue, diethyl ether was added
  3. custominsoluble matter was separated by filtration

출처 및 근거

ORD 기록
ord-8e705ba5bc344863b0bd715a0f1ae6f4
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09206173B2

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