Isopropanol → Isopropyl 2-Chloro-4-Trifluoromethyl-5-Thiazolecarboxylate

HRID 2049934ノート

反応式

HRID 2049934 の反応式
[Cl:1][C:2]1[S:3][C:4]([C:11](Cl)=[O:12])=[C:5]([C:7]([F:10])([F:9])[F:8])[N:6]=1.[CH:14]([OH:17])([CH3:16])[CH3:15]>>[Cl:1][C:2]1[S:3][C:4]([C:11]([O:17][CH:14]([CH3:16])[CH3:15])=[O:12])=[C:5]([C:7]([F:8])([F:9])[F:10])[N:6]=1

参加物

3

反応物 2

HCID 3776IsopropanolHCID 132827442-Chloro-4-trifluoromethyl-5-thiazolecarbonyl chloride

生成物 1

HCID 13282745Isopropyl 2-Chloro-4-Trifluoromethyl-5-Thiazolecarboxylate収率 86.1%

実験手順

The acid chloride of Example 16 (5.2 g), and 10 g of isopropanol were held at reflux for 16 hours. Excess alcohol was removed under reduced pressure. The residue was dissolved in 50 ml. of ether. The ether solution was washed with sodium bicarbonate, dried (MgSO4) and concentrated under reduced pressure. The crude product was distilled at 1 mm. on a Kugelrohr to give 4.9 g (86%) of the desired product as colorless liquid, nD25 =1.4655.

後処理

  1. temperatureat reflux for 16 hours
  2. customExcess alcohol was removed under reduced pressure
  3. dissolutionThe residue was dissolved in 50 ml
  4. washThe ether solution was washed with sodium bicarbonate
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated under reduced pressure
  7. distillationThe crude product was distilled at 1 mm

出典と根拠

ORDレコード
ord-583b7ab5798d4539847396c5f03105d9
出典データセット
uspto-grants-1980_04
特許番号
US04199506

反応ノート

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