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Sodium Hydroxide → 3-(4-Methoxybenzylmercapto)-4-n-butyl-1,2,4-triazole

HRID 1112108
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HRID 1112108 반응식
[SH:1][C:2]1[N:6]([CH2:7][CH2:8][CH2:9][CH3:10])[CH:5]=[N:4][N:3]=1.[OH-].[Na+].[CH3:13][O:14][C:15]1[CH:22]=[CH:21][C:18]([CH2:19]Cl)=[CH:17][CH:16]=1>CO>[CH3:13][O:14][C:15]1[CH:22]=[CH:21][C:18]([CH2:19][S:1][C:2]2[N:6]([CH2:7][CH2:8][CH2:9][CH3:10])[CH:5]=[N:4][N:3]=2)=[CH:17][CH:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 699934-Methyloxybenzyl chlorideHCID 178448642HCID 178448642, 화합물

생성물 1

HCID 128884523-(4-Methoxybenzylmercapto)-4-n-butyl-1,2,4-triazole

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a mixture of 10 g. (0.064 mole) of 3-mercapto-4-n-butyl-1,2,4-triazole and 2.6 g. (0.064 mole) of sodium hydroxide in 200 ml. of methanol was added 9.9 g. (0.064 mole) of p-methoxybenzyl chloride. The reaction mixture was heated at reflux about 20 hours. The solvent was evaporated off, the residue washed with water, dried and distilled. There was obtained 17.8 g. of yellow liquid distilling at 190°-205° C. at 0.03 mm. Nuclear magnetic resonance and ultraviolet spectra indicated this to be approximately an equal mixture of 3-(4-methoxybenzylmercapto)-4-n-butyl-1,2,4-triazole and 4-n-butyl-2-(4-methoxybenzyl)-1,2,4-triazoline-3-thione.

후처리

  1. additionTo a mixture of 10 g
  2. temperatureThe reaction mixture was heated
  3. temperatureat reflux about 20 hours
  4. customThe solvent was evaporated off
  5. washthe residue washed with water
  6. customdried
  7. distillationdistilled
  8. customThere was obtained 17.8 g
  9. distillationof yellow liquid distilling at 190°-205° C. at 0.03 mm
  10. additionan equal mixture of 3-(4-methoxybenzylmercapto)-4-n-butyl-1,2,4-triazole and 4-n-butyl-2-(4-methoxybenzyl)-1,2,4-triazoline-3-thione

출처 및 근거

ORD 기록
ord-ebbb97db9f5c4841bd5f21355d8c6d9e
출처 데이터셋
uspto-grants-1978_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04120864

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