1,2,4-Triazolylsodium → 1-(N-(2-isopropylvinyl)-N-tert.-butylcarbamoyl)-1,2,4-triazole

HRID 1762856노트

반응식

HRID 1762856 반응식
[CH:1]([CH:4]=[CH:5][N:6]([C:10]([CH3:13])([CH3:12])[CH3:11])[C:7](Cl)=[O:8])([CH3:3])[CH3:2].[NH:14]1[CH:18]=[N:17][C-:16]=[N:15]1.[Na+]>O1CCCC1>[CH:1]([CH:4]=[CH:5][N:6]([C:10]([CH3:13])([CH3:12])[CH3:11])[C:7]([N:14]1[CH:18]=[N:17][CH:16]=[N:15]1)=[O:8])([CH3:3])[CH3:2]

참가 물질

4

반응물 2

HCID 547199651,2,4-TriazolylsodiumHCID 56617464N-(2-isopropylvinyl)-N-tert.-butylcarbamyl chloride

생성물 1

HCID 566067651-(N-(2-isopropylvinyl)-N-tert.-butylcarbamoyl)-1,2,4-triazole수율 55.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
65 °C

실험 절차

21 g (0.103 mole) of N-(2-isopropylvinyl)-N-tert.-butylcarbamyl chloride are added dropwise to a suspension of 10.5 g (0.115 mole) of sodium 1,2,4-triazolide in 100 ml of dry tetrahydrofuran at 20° C. The mixture is stirred for 6 hours at 65° C., after which it is cooled to 20° C., the resulting precipitate is filtered off under suction, the filtrate is evaporated down and the oil which remains is distilled under reduced pressure. 13.6 g of 1-(N-(2-isopropylvinyl)-N-tert.-butylcarbamoyl)-1,2,4-triazole are obtained as a colorless liquid of boiling point 95°-97° C./0.15 mbar and nD 1.4815 (Compound No. 2)

후처리

  1. temperatureafter which it is cooled to 20° C.
  2. filtrationthe resulting precipitate is filtered off under suction
  3. customthe filtrate is evaporated down
  4. distillationthe oil which remains is distilled under reduced pressure

출처 및 근거

ORD 기록
ord-b55449881a2146afa5550dec17bf16e3
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04835171

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