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Ethyl bromoacetate → Ethyl 1H-1,2,4-triazole-1-acetate

HRID 64064
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HRID 64064 반응식
[NH:1]1[CH:5]=[N:4][CH:3]=[N:2]1.C([O-])([O-])=O.[K+].[K+].Br[CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15]>CN(C=O)C>[N:1]1([CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH:5]=[N:4][CH:3]=[N:2]1
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참가 물질

5

반응물 3

HCID 7748Ethyl bromoacetateHCID 92571H-1,2,4-TriazoleHCID 11430Potassium Carbonate

생성물 1

HCID 557521Ethyl 1H-1,2,4-triazole-1-acetate수율 65%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 1H-1,2,4-triazol (2 g, 29.9 mmol, 1.0 eq) in DMF were added K2CO3 (12.3 g, 88.9 mmol, 3 eq.) and ethyl 2-bromoacetate (4.8 g, 29.9 mmol, 1 eq). The mixture was stirred at RT for 16 h. The mixture was quenched and extracted as in Intermediate Example 5(a). The solvent was distilled off to give the product in 65% yield (3 g). LC-MS (ESI): Calculated mass: 155.0; Observed mass: 156.1 [M+H]+ (rt: 0.113 min).

후처리

  1. customThe mixture was quenched
  2. extractionextracted as in Intermediate Example 5(a)
  3. distillationThe solvent was distilled off
  4. customto give the product in 65% yield (3 g)
  5. custom156.1 [M+H]+ (rt: 0.113 min)

출처 및 근거

ORD 기록
ord-509fe4691649464e92776e45b5ffda9f
출처 데이터셋
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09447091B2

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