N-甲基吗啉 → ((5-Isoxazolyl)methyl)-(4-nitrophenyl)carbonate

HRID 52844笔记

反应方程式

HRID 52844 反应方程式
[N+:1]([C:4]1[CH:13]=[CH:12][C:7]([O:8][C:9](Cl)=[O:10])=[CH:6][CH:5]=1)([O-:3])=[O:2].[OH:14][CH2:15][C:16]1[O:20][N:19]=[CH:18][CH:17]=1.CN1CCOCC1>C(Cl)Cl>[N+:1]([C:4]1[CH:13]=[CH:12][C:7]([O:8][C:9]([O:14][CH2:15][C:16]2[O:20][N:19]=[CH:18][CH:17]=2)=[O:10])=[CH:6][CH:5]=1)([O-:3])=[O:2]

参与物

5

反应物 3

HCID 7972N-甲基吗啉HCID 82129对硝基苯基氯甲酸酯HCID 129050985-羟甲基异恶唑

产物 1

HCID 18939817((5-Isoxazolyl)methyl)-(4-nitrophenyl)carbonate

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂3 次

实验过程

A 631 mg (2.65 mmol) sample of p-nitrophenoxycarbonylchloride in 2 mL of methylene chloride was added to a solution of 310 mg (3.13 mmol) of 5-hydroxymethyisoxazole and 0.344 mL of 4-methylmorpholine in 2 mL of methylene chloride cooled in an ice bath. The solution was stirred for 4 hours. The mixture was diluted with methylene chloride, which was washed with water, dried and concentrated. The crude product was chromatographed on silica gel, eluting with 2% ethyl acetate in methylene chloride. The solvent was removed and the product dried to afford 0.473 g of the title compound, which was taken directly to the next step.

后处理

  1. temperaturecooled in an ice bath
  2. washwas washed with water
  3. customdried
  4. concentrationconcentrated
  5. customThe crude product was chromatographed on silica gel
  6. washeluting with 2% ethyl acetate in methylene chloride
  7. customThe solvent was removed
  8. customthe product dried

来源与证据

ORD记录
ord-45bff5541a6445968c497a9102844961
来源数据集
uspto-grants-1997_04
专利号
US05616714

反应笔记

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