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

HRID 2094318
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HRID 2094318 반응식
[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]
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참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 1140Toluene용매
HCID 8028
Tetrahydrofuran
용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5c52d04752434d8795be15a4d5d4ad64
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08445525B2

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