Phosphorus oxychloride → Ethyl-2-methoxymethyl-4-chloropyrimidine-5-acetate

반응식

[CH3:1][O:2][CH2:3][C:4]1[N:9]=[C:8](O)[C:7]([CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:6][N:5]=1.P(Cl)(Cl)([Cl:19])=O>>[CH2:15]([O:14][C:12](=[O:13])[CH2:11][C:7]1[C:8]([Cl:19])=[N:9][C:4]([CH2:3][O:2][CH3:1])=[N:5][CH:6]=1)[CH3:16]

참가 물질

반응물 2

HCID 24813Phosphorus oxychloride

HCID 178470733HCID 178470733, 화합물

생성물 1

HCID 19066271Ethyl-2-methoxymethyl-4-chloropyrimidine-5-acetate수율 78%

실험 절차

A mixture of the product of Step 1, above (0.01 mol) and phosphorous oxychloride (7 ml) was refluxed for 20 minutes. The excess phosphorous oxychloride was removed, the residue was quenched with ice water (15 ml) and the mixture was extracted with ethyl acetate (2×20 ml). The ethyl acetate layer was collected and washed with water (2×10 ml). The organic extract was collected, dried over MgSO4 and the dried portion was evaporated to obtain the title compound as an oil (78% yield).

후처리

customThe excess phosphorous oxychloride was removed
customthe residue was quenched with ice water (15 ml)
extractionthe mixture was extracted with ethyl acetate (2×20 ml)
customThe ethyl acetate layer was collected
washwashed with water (2×10 ml)
extractionThe organic extract
customwas collected
dry with materialdried over MgSO4
customthe dried portion was evaporated

출처 및 근거

ORD 기록: ord-7d69c9c0cd244e8aa1776baa6ae8f9ea
출처 데이터셋: uspto-grants-1998_08
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US05789415

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