Cesium carbonate → 2-Methylthio-4-(ethoxycarbonylmethyl)amino-5-nitro-6-(3-(dimethylaminocarbonyl)-phenoxy)pyrimidine

HRID 1456951노트

반응식

HRID 1456951 반응식
[CH3:1][S:2][C:3]1[N:8]=[C:7](Cl)[C:6]([N+:10]([O-:12])=[O:11])=[C:5]([O:13][C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([C:20]([N:22]([CH3:24])[CH3:23])=[O:21])[CH:15]=2)[N:4]=1.Cl.[CH2:26]([O:28][C:29](=[O:32])[CH2:30][NH2:31])[CH3:27].C(=O)([O-])[O-].[Cs+].[Cs+]>C(#N)C>[CH3:1][S:2][C:3]1[N:8]=[C:7]([NH:31][CH2:30][C:29]([O:28][CH2:26][CH3:27])=[O:32])[C:6]([N+:10]([O-:12])=[O:11])=[C:5]([O:13][C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([C:20]([N:22]([CH3:24])[CH3:23])=[O:21])[CH:15]=2)[N:4]=1

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 2723640Glycine ethyl ester, hydrochlorideHCID 221026862-Methylthio-4-chloro-5-nitro-6-(3-dimethylaminocarbonylphenoxy)pyrimidine

생성물 1

HCID 221033402-Methylthio-4-(ethoxycarbonylmethyl)amino-5-nitro-6-(3-(dimethylaminocarbonyl)-phenoxy)pyrimidine

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To 2-methylthio-4-chloro-5-nitro-6-(3-(dimethylaminocarbonyl)phenoxy)pyrimidine, a compound of formula (C), (3.0 g 8.14 mmol) in 80 mL of acetonitrile at 0° C. was added glycine ethyl ester hydrochloride, a compound of formula (D), (1.14 g, 8.14 mmol), followed by the addition of cesium carbonate (6.1 g, 18.7 mmol). The reaction mixture was allowed to warm to ambient temperature and then stirred for 2 hours. The volatiles were evaporated to yield 3.6 g of 2-methylthio-4-(ethoxycarbonylmethyl)amino-5-nitro-6-(3-(dimethylaminocarbonyl)-phenoxy)pyrimidine, a compound of formula (E).

후처리

  1. customThe volatiles were evaporated

출처 및 근거

ORD 기록
ord-18290c507c3b461d9fb521c1822818fb
출처 데이터셋
uspto-grants-1998_12
특허 번호
US05846972

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