2-Aminothiophenol → 2,2'-Propane-2,2-diylbis(1,3-benzothiazole)

HRID 1471236

반응식

HRID 1471236 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[SH:8].[CH3:9][C:10]([CH3:17])([C:14](O)=O)[C:11](O)=O>O>[CH3:9][C:10]([C:14]1[S:8][C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[N:1]=1)([C:17]1[S:8][C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[N:1]=1)[CH3:11]

참가 물질

4

반응물 2

HCID 87132-AminothiophenolHCID 11686Dimethylmalonic acid

생성물 1

HCID 117818732,2'-Propane-2,2-diylbis(1,3-benzothiazole)

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a flask were added 50 g polyphosphoric acid. After heating to 70 C under nitrogen, a mixture of 3.13 g 2-aminothiophenol and 1.65 g dimethylmalonic acid was added. The reaction mixture was heated to 150 C for 2 hours, then 165 C for 3 hours. After cooling to 80 C, the mixture was poured into 100 ml water. The slurry was cooled to 5 C, filtered and the solid was washed with water. The solid was added to a mixture of 20 ml ethanol and 210 ml water at 50 C and basified with aqueous ammonium hydroxide. After cooling to 10 C, the solid was filtered and washed with water. The solid was dissolved in 50 ml hot ethanol, hot filtered and 5 ml water was added and the solution was cooled to 5 C. Following filtration, the white solid was washed with 75% ethanol and dried.

후처리

  1. temperatureAfter heating to 70 C under nitrogen
  2. additionwas added
  3. temperatureThe reaction mixture was heated to 150 C for 2 hours
  4. temperatureAfter cooling to 80 C
  5. temperatureThe slurry was cooled to 5 C
  6. filtrationfiltered
  7. washthe solid was washed with water
  8. additionThe solid was added to a mixture of 20 ml ethanol and 210 ml water at 50 C
  9. temperatureAfter cooling to 10 C
  10. filtrationthe solid was filtered
  11. washwashed with water
  12. dissolutionThe solid was dissolved in 50 ml hot ethanol
  13. filtrationhot filtered
  14. addition5 ml water was added
  15. temperaturethe solution was cooled to 5 C
  16. filtrationfiltration
  17. washthe white solid was washed with 75% ethanol
  18. customdried

출처 및 근거

ORD 기록
ord-9d7e591e523e488e924c12e378132db1
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09011734B2

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