二氯甲烷 → HCID 20061639，化合物

HRID 1650737笔记

反应方程式

HRID 1650737 反应方程式
[O:1]=[C:2]1[NH:6][C:5]([C:7]([F:10])([F:9])[F:8])=[C:4]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[S:3]1.[H-].[Na+].P(O)(O)([O-])=O.[Na+].C(Cl)Cl.O1C[CH2:30][CH2:29][CH2:28]1>>[O:1]=[C:2]1[N:6]([CH2:30][C:29]#[CH:28])[C:5]([C:7]([F:8])([F:9])[F:10])=[C:4]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[S:3]1

参与物

6

反应物 5

HCID 6344二氯甲烷HCID 8028四氢呋喃HCID 24758氢化钠HCID 27830412-羟基-4-(三氟甲基)噻唑-5-羧酸乙酯HCID 23672064磷酸二氢钠

产物 1

HCID 20061639HCID 20061639，化合物

实验过程

6.9 g of ethyl 2,3-dihydro-2-oxo-4-trifluoromethyl-5-thiazole-carboxylate [prepared by the process of CA 92 110 998P] were dissolved in 70 ml of tetrahydrofuran at 0° ± 5° C. and then, 1.44 g of 50% sodium hydride in oil were added. Once the gaseous evolution ended, 15 ml of 2-bromopropyne were added and the mixture was refluxed for 48 hours. The mixture was poured on to an iced solution of monosodium phosphate and extraction was carried out with methylene chloride, then drying, filtering and concentrating under reduced pressure. The residue was chromatographed and elution with a hexane-ethyl acetate mixture (85-15) yielded 5.57 g of the expected product.

后处理

  1. temperaturethe mixture was refluxed for 48 hours
  2. customdrying
  3. filtrationfiltering
  4. concentrationconcentrating under reduced pressure
  5. customThe residue was chromatographed
  6. washelution with a hexane-ethyl acetate mixture (85-15)

来源与证据

ORD记录
ord-362c344b7ca244068ee05b746f92ef4f
来源数据集
uspto-grants-1990_05
专利号
US04925862

反应笔记

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