Phosphorus oxychloride → 3-Chloro-6-methoxypyrazin-2-amine

반응식

[NH2:1][C:2]1[CH:7]=[N+:6]([O-])[CH:5]=[C:4]([O:9][CH3:10])[N:3]=1.P(Cl)(Cl)([Cl:13])=O>>[NH2:1][C:2]1[C:7]([Cl:13])=[N:6][CH:5]=[C:4]([O:9][CH3:10])[N:3]=1

참가 물질

반응물 2

HCID 24813Phosphorus oxychloride

HCID 205289822-Amino-6-methoxypyrazine 4-oxide

생성물 1

HCID 117010873-Chloro-6-methoxypyrazin-2-amine

실험 절차

A suspension of 2-amino-6-methoxypyrazine 4-oxide in freshly distilled phosphorus oxychloride is refluxed for one hour. Thin layer chromatography indicates that the starting material is no longer present. The excess of phosphorus oxychloride is removed in vacuo and the residue is treated with crushed ice. If decomposition is complete the solution is made alkaline with 10% sodium hydroxide and extracted with chloroform. The chloroform extracts are washed with water, dried over sodium sulfate and evaporated to give the product which may be recrystallized from a suitable solvent such as ethanol.

후처리

temperatureis refluxed for one hour
customThe excess of phosphorus oxychloride is removed in vacuo
additionthe residue is treated with crushed ice
extractionextracted with chloroform
washThe chloroform extracts are washed with water
dry with materialdried over sodium sulfate
customevaporated
customto give the product which
custommay be recrystallized from a suitable solvent such as ethanol

출처 및 근거

ORD 기록: ord-d21f8adf8297470da7103afcdb971758
출처 데이터셋: uspto-grants-1977_08
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04042586

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