Ethyl 3-bromopropionate → Ethyl-3-(5-p-tolyl-2-tetrazolyl)propionate

HRID 584128노트

반응식

HRID 584128 반응식
[O-]CC.[Na+].[C:5]1([CH3:16])[CH:10]=[CH:9][C:8]([C:11]2[NH:15][N:14]=[N:13][N:12]=2)=[CH:7][CH:6]=1.Br[CH2:18][CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21]>C(O)C>[CH2:23]([O:22][C:20](=[O:21])[CH2:19][CH2:18][N:13]1[N:14]=[N:15][C:11]([C:8]2[CH:7]=[CH:6][C:5]([CH3:16])=[CH:10][CH:9]=2)=[N:12]1)[CH3:24]

참가 물질

5

반응물 3

HCID 68320Ethyl 3-bromopropionateHCID 2723922Sodium ethoxideHCID 178424083HCID 178424083, 화합물

생성물 1

HCID 22343049Ethyl-3-(5-p-tolyl-2-tetrazolyl)propionate

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Sodium ethoxide (21%, 173 μL, 0.536 mmol) was dissolved in 650 μL absolute ethanol along with 5-p-tolyl tetrazole (65.9 mmol) at reflux. Ethyl 3-bromo-propionate (69 μL, 0.536 mmol) was added at reflux and the mixture was maintained at reflux overnight. The crude mixtures were filtered, concentrated and extracted with diethyl ether and sat. NaHCO3. The organic layers were dried and evaporated. When necessary, further purification was performed by RP-HPLC to provide ethyl-3-(5-p-tolyl-2-tetrazolyl)propionate.

후처리

  1. temperatureat reflux
  2. temperatureat reflux
  3. temperaturethe mixture was maintained
  4. temperatureat reflux overnight
  5. filtrationThe crude mixtures were filtered
  6. concentrationconcentrated
  7. extractionextracted with diethyl ether and sat. NaHCO3
  8. customThe organic layers were dried
  9. customevaporated
  10. customWhen necessary, further purification

출처 및 근거

ORD 기록
ord-21b2eadddd8645418a57c6164dd89393
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06924284B2

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