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Methanethiol → HCID 178503578, 화합물

HRID 1580433
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HRID 1580433 반응식
[CH3:1][SH:2].[CH:3]([N:6]1[C:10](Cl)=[N:9][C:8]([OH:12])=[N:7]1)([CH3:5])[CH3:4].S([O-])(O)(=O)=O.[K+]>[OH-].[Na+]>[CH:3]([N:6]1[C:10]([S:2][CH3:1])=[N:9][C:8]([OH:12])=[N:7]1)([CH3:5])[CH3:4]
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참가 물질

5

반응물 3

HCID 878MethanethiolHCID 516920Potassium bisulfateHCID 178456690HCID 178456690, 화합물

생성물 1

HCID 178503578HCID 178503578, 화합물

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

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온도
100 °C

실험 절차

An amount of 19.6 g of methylmercaptan is added at -5°C, with stirring, to 200 ml of 5N aqueous sodium hydroxide solution. An addition is then made of 33 g of 1-isopropyl-5-chloro-3-hydroxy-1,2,4-triazole, and the mixture heated for 2 hours at 100°C. After cooling to 20°C, the solution is acidified by the addition of potassium hydrogen sulphate, and extracted with ethyl acetate. The ethyl acetate extract is dried over anhydrous magnesium sulphate; it is then concentrated in a water-jet vacuum, and the residue crystallised from a little methanol at -70°C. The obtained product is 1-isopropyl-5-methylmercapto-3-hydroxy-1,2,4-triazole with a melting point of 90°-92°C.

후처리

  1. additionAn addition
  2. temperatureAfter cooling to 20°C
  3. extractionextracted with ethyl acetate
  4. extractionThe ethyl acetate extract
  5. dry with materialis dried over anhydrous magnesium sulphate
  6. concentrationit is then concentrated in a water-jet vacuum
  7. customthe residue crystallised from a little methanol at -70°C

출처 및 근거

ORD 기록
ord-803df289c435420881cd8a952d478534
출처 데이터셋
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03932630

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