Triethylamine → HCID 178488517, 화합물

HRID 1517395노트

반응식

HRID 1517395 반응식
[NH:1]1[CH:5]=[N:4][CH:3]=[N:2]1.P(Cl)(Cl)(Cl)=O.[C:11]([NH:14][C:15]1[NH:16][C:17](=O)[C:18]2[N:24]=[C:23]([C:25]3[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[C:27]([O:33][CH3:34])[CH:26]=3)[CH:22]=[CH:21][C:19]=2[N:20]=1)(=[O:13])[CH3:12].C(N(CC)CC)C>C(#N)C>[C:11]([NH:14][C:15]1[N:16]=[C:17]([C:5]2[N:4]=[CH:3][NH:2][N:1]=2)[C:18]2[N:24]=[C:23]([C:25]3[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[C:27]([O:33][CH3:34])[CH:26]=3)[CH:22]=[CH:21][C:19]=2[N:20]=1)(=[O:13])[CH3:12]

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 92571H-1,2,4-TriazoleHCID 24813Phosphorus oxychlorideHCID 136389259HCID 136389259, 화합물

생성물 1

HCID 178488517HCID 178488517, 화합물수율 91.6%

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

A suspension of 1,2,4-triazole (8.28 g, 120 mmol) and phosphorus oxychloride (3.2 ml, 36 mmol) in dry acetonitrile (150 ml) was added to a stirred suspension of 2-acetamido-6-(3,4-dimethoxyphenyl)pyrido[3,2-d]pyrimidin-4(3H)-one (4.08 g, 12 mmol) and triethylamine (5.2 ml, 36 mmol) in dry acetonitrile (150 ml). The mixture was stirred at room temperature under nitrogen for 3 days and the yellow precipitate was filtered off, then successively washed with ethanol and ether, and dried over P2O5 in a vacuum dessicator resulting in the pure title compound (4.3 g, yield 90%) which was characterized by its mass spectrum as follows: MS (m/z): 392 ([M+H]+, 100), 414 ([M+Na]+; 804 [2M+Na]+

후처리

  1. filtrationthe yellow precipitate was filtered off
  2. washsuccessively washed with ethanol and ether
  3. dry with materialdried over P2O5 in a vacuum dessicator

출처 및 근거

ORD 기록
ord-8fa9863b2fdb4cffacd5668e574c6cbb
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08232278B2

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