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Hydrochloric Acid → Triazamate acid

HRID 1252157
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인쇄 미리보기

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HRID 1252157 반응식
[CH3:1][N:2]([CH3:21])[C:3]([N:5]1[C:9]([S:10][CH2:11][C:12]([O:14]CC)=[O:13])=[N:8][C:7]([C:17]([CH3:20])([CH3:19])[CH3:18])=[N:6]1)=[O:4].Cl>C1COCC1>[CH3:1][N:2]([CH3:21])[C:3]([N:5]1[C:9]([S:10][CH2:11][C:12]([OH:14])=[O:13])=[N:8][C:7]([C:17]([CH3:19])([CH3:18])[CH3:20])=[N:6]1)=[O:4]
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 86306Triazamate

생성물 1

HCID 14299898Triazamate acid

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
20 °C

실험 절차

To 1.2 g of 1-dimethylcarbamoyl-3-t-butyl-5-carboethoxymethylthio-1H-1,2,4-triazole (the compound of Example 2) in 20 ml of THF was added 4 ml of 12M HCl. After stirring for 48 h at 20° C. the reaction mixture was partitioned between ether and water, the ether layer was extracted with dilute NaOH and the resulting aqueous layer was acidified and extracted with fresh ether. The resulting ether layer was dried over magnesium sulfate, filtered and evaporated under vacuum to yield 1-dimethylcarbamoyl-3-t-butyl-5-carboxymethylthio-1H-1,2,4-triazole as an oil.

후처리

  1. customwas partitioned between ether and water
  2. extractionthe ether layer was extracted with dilute NaOH
  3. extractionextracted with fresh ether
  4. dry with materialThe resulting ether layer was dried over magnesium sulfate
  5. filtrationfiltered
  6. customevaporated under vacuum

출처 및 근거

ORD 기록
ord-1d7b0b845d974955b99d01aaaf83b577
출처 데이터셋
uspto-grants-1988_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04742072

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