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Water → Ethyl 3-chloro-4-(4-methyl-2-oxo-oxazolidin-3-yl)-benzoate

HRID 551241
ノート
印刷プレビュー

反応式

HRID 551241 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][C:12]=1[NH:13][CH:14]([CH3:17])[CH2:15][OH:16])[C:5]([O:7][CH2:8][CH3:9])=[O:6].C(N(CC)CC)C.[C:25](Cl)(Cl)=[O:26].O>C1COCC1.C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][C:12]=1[N:13]1[CH:14]([CH3:17])[CH2:15][O:16][C:25]1=[O:26])[C:5]([O:7][CH2:8][CH3:9])=[O:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 6371PhosgeneHCID 8471TriethylamineHCID 67048695Ethyl 3-chloro-4-(2-hydroxy-1-methyl-ethylamino)-benzoate

生成物 1

HCID 67048447Ethyl 3-chloro-4-(4-methyl-2-oxo-oxazolidin-3-yl)-benzoate

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒
HCID 8028
Tetrahydrofuran
溶媒

実験手順

0.50 g (1.94 mmol) ethyl 3-chloro-4-(2-hydroxy-1-methyl-ethylamino)-benzoate are placed in 30 ml THF together with 0.22 g (2.20 mmol) triethylamine and 1.10 ml (2.08 mmol) 20% phosgene solution in toluene is added with stirring at ambient temperature. The mixture is stirred for 1 hour at ambient temperature, then 1 ml of water is added and the mixture is stirred for another 10 minutes. The mixture is then evaporated down i. vac., combined with water and extracted with ethyl acetate. The combined organic phases are washed with water and sat. sodium chloride solution, dried over sodium sulphate and evaporated down i. vac.

後処理

  1. additionis added
  2. stirringThe mixture is stirred for 1 hour at ambient temperature
  3. stirringthe mixture is stirred for another 10 minutes
  4. customThe mixture is then evaporated down i
  5. extractionextracted with ethyl acetate
  6. washThe combined organic phases are washed with water and sat. sodium chloride solution
  7. dry with materialdried over sodium sulphate
  8. customevaporated down i

出典と根拠

ORDレコード
ord-02a19416b1964116af89c36771e496ad
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07947700B2

反応ノート

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