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Formic Acid → Ethyl 1-(2-Hydroxyethyl)-1,2,3-triazole-4-carboxylate

HRID 1650131
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HRID 1650131 반응식
[CH2:1]([CH2:3][NH2:4])[OH:2].C(O)=O.[CH:8]([C:10](=[N+:16]=[N-:17])[C:11]([O:13][CH2:14][CH3:15])=[O:12])=O>CO>[OH:2][CH2:1][CH2:3][N:4]1[CH:8]=[C:10]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[N:16]=[N:17]1
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참가 물질

5

반응물 3

HCID 284Formic AcidHCID 700EthanolamineHCID 54182403Ethyl 2-diazo-2-formylacetate

생성물 1

HCID 23048708Ethyl 1-(2-Hydroxyethyl)-1,2,3-triazole-4-carboxylate수율 74.9%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

A solution of ethanolamine (60 ml, 1 mole) in methanol (320 ml) at 5° was treated with formic acid until a pH of 5 was obtained. A solution of ethyl α-formyldiazoacetate (crude, approximately 0.3 mole) in methanol (320 ml) was then added and the mixture stirred at room temperature for two days. The mixture was then evaporated, chloroform (1 liter), then water (200 ml) was added and the mixture was treated with sodium bicarbonate until a pH of 7 was reached. The phases were separated and the aqueous phase saturated with sodium chloride and extracted with chloroform (6×300 ml). The combined organic phases were dried (MgSO4), filtered and evaporated. The residue was then dissolved in toluene (approximately 100 ml). The resulting crystalline solid was filtered, washed with ether and dried to provide the title compound (41.6 g) as a solid; υmax (nujol) 3320, 3140, 1725 cm-1 ; δ (CDCl3), 1.38 (3H, t, J 7.5 Hz), 4.00-4.80 (7H, m, becomes 6H, m on D2O exch), 8.40 (1H, s). This material was pure enough for further synthetic progression.

후처리

  1. customwas obtained
  2. customThe mixture was then evaporated
  3. additionchloroform (1 liter), then water (200 ml) was added
  4. additionthe mixture was treated with sodium bicarbonate until a pH of 7
  5. customThe phases were separated
  6. extractionthe aqueous phase saturated with sodium chloride and extracted with chloroform (6×300 ml)
  7. dry with materialThe combined organic phases were dried (MgSO4)
  8. filtrationfiltered
  9. customevaporated
  10. dissolutionThe residue was then dissolved in toluene (approximately 100 ml)
  11. filtrationThe resulting crystalline solid was filtered
  12. washwashed with ether
  13. customdried

출처 및 근거

ORD 기록
ord-73728510956b4b8e8e106dd781a191aa
출처 데이터셋
uspto-grants-1990_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04923856

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