Dichloromethane → HCID 20061639、化合物

HRID 1650737ノート

反応式

HRID 1650737 の反応式
[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

参加物

6

反応物 5

HCID 6344DichloromethaneHCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 2783041Ethyl 2-oxo-4-(trifluoromethyl)-2,3-dihydro-1,3-thiazole-5-carboxylateHCID 23672064Monosodium phosphate

生成物 1

HCID 20061639HCID 20061639、化合物

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-362c344b7ca244068ee05b746f92ef4f
出典データセット
uspto-grants-1990_05
特許番号
US04925862

反応ノート

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