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Ethyl chloroformate → 2-Chloro-4-(3-trifluoromethyl-phenyl)-thiazole-5-carboxylic acid ethyl ester

HRID 1667672
ノート
印刷プレビュー

反応式

HRID 1667672 の反応式
[Cl:1][C:2]1[S:3][CH:4]=[C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([C:13]([F:16])([F:15])[F:14])[CH:8]=2)[N:6]=1.C([Li])CCC.Cl[C:23]([O:25][CH2:26][CH3:27])=[O:24]>O1CCCC1>[CH2:26]([O:25][C:23]([C:4]1[S:3][C:2]([Cl:1])=[N:6][C:5]=1[C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([C:13]([F:16])([F:14])[F:15])[CH:8]=1)=[O:24])[CH3:27]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 10928Ethyl chloroformateHCID 629425372-Chloro-4-(3-trifluoromethyl-phenyl)-thiazoleHCID 178418339Butyllithium

生成物 1

HCID 130418212-Chloro-4-(3-trifluoromethyl-phenyl)-thiazole-5-carboxylic acid ethyl ester収率 43.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 10.1 g (38.3 mmole) of 2-chloro-4-(3-trifluoromethyl-phenyl)-thiazole in 120 mL of tetrahydrofuran at −78 degrees was added over 20 minutes, 20 mL of 2.5 M n-butyl lithium in hexanes. The mixture was stirred for 2 hours and then 19 mL (93.4 mmole) of ethyl chloroformate was added quickly. The mixture was stirred for 15 minutes, then the cooling bath was removed. After 25 minutes, the reaction was quenched by the addition of 150 mL of 1M hydrochloric acid. The mixture was stirred for 5 minutes, and then diluted with 1 L of ethyl acetate. The ethyl acetate layer was washed twice with 150 mL of water, once with 100 mL of brine, dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. The residue was purified by silica gel chromatography, eluting with dichloromethane-hexanes (gradient 10:90-50:50) to give 5.62 g of 2-chloro-4-(3-trifluoromethyl-phenyl)-thiazole-5-carboxylic acid ethyl ester as a golden oil.

後処理

  1. stirringThe mixture was stirred for 15 minutes
  2. customthe cooling bath was removed
  3. waitAfter 25 minutes
  4. customthe reaction was quenched by the addition of 150 mL of 1M hydrochloric acid
  5. stirringThe mixture was stirred for 5 minutes
  6. additiondiluted with 1 L of ethyl acetate
  7. washThe ethyl acetate layer was washed twice with 150 mL of water, once with 100 mL of brine
  8. dry with materialdried over anhydrous sodium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated under reduced pressure
  11. customThe residue was purified by silica gel chromatography
  12. washeluting with dichloromethane-hexanes (gradient 10:90-50:50)

出典と根拠

ORDレコード
ord-d3e0f0a3c15d4624aa64ce3bd2892554
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08044213B2

反応ノート

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