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Ethyl 2-bromopropionate → HCID 13909862, 화합물

HRID 1194630
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HRID 1194630 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]=[C:9]2[N:17]3[N:12]([CH2:13][CH2:14][CH2:15][CH2:16]3)[C:11](=[O:18])[S:10]2)=[CH:4][C:3]=1[NH2:19].Br[CH:21]([CH3:27])[C:22]([O:24][CH2:25][CH3:26])=[O:23].C(=O)([O-])O.[Na+]>>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]=[C:9]2[N:17]3[N:12]([CH2:13][CH2:14][CH2:15][CH2:16]3)[C:11](=[O:18])[S:10]2)=[CH:4][C:3]=1[NH:19][CH:21]([C:22]([O:24][CH2:25][CH3:26])=[O:23])[CH3:27]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 79040Ethyl 2-bromopropionateHCID 516892Sodium BicarbonateHCID 19987017HCID 19987017, 화합물

생성물 1

HCID 13909862HCID 13909862, 화합물수율 52%

실험 절차

Into a reaction flask equipped with a Dimroth condenser, 2.2 g (7.4 mmol) of 9-(4-chloro-3-aminophenylimino)-8-thia-1,6-diazabicyclo[4.3.0]nonane-7-one, 15 ml of ethyl 2-bromopropionate and 2.0 g (24 mmol) of sodium hydrogen carbonate, were charged, and refluxed under heating for 4 hours to complete the reaction. The reaction solution was filtered, concentrated and extracted with ethyl acetate, and then washed with water and dried over anhydrous sodium sulfate. The solvent was distilled off to obtain a crude product, which was purified by column chromatography to obtain 1.5 g (yield: 52%) of colorless oily substance. Refractive index: nD20 1.5755

후처리

  1. additionwere charged
  2. temperaturerefluxed
  3. temperatureunder heating for 4 hours
  4. customthe reaction
  5. filtrationThe reaction solution was filtered
  6. concentrationconcentrated
  7. extractionextracted with ethyl acetate
  8. washwashed with water
  9. dry with materialdried over anhydrous sodium sulfate
  10. distillationThe solvent was distilled off

출처 및 근거

ORD 기록
ord-3acc311a7e154de88a54a1b496e201c7
출처 데이터셋
uspto-grants-1989_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04816063

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