Hydrochloric Acid → HCID 21107906, 화합물

HRID 1765962노트

반응식

HRID 1765962 반응식
[C:1]1([C:7]2[C:8]([NH2:20])=[C:9]([NH2:19])[C:10]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)=[CH:11][CH:12]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:21](O)(=O)[CH:22]([CH3:24])[OH:23].Cl>>[C:13]1([C:10]2[C:9]3[N:19]=[C:21]([CH:22]([OH:23])[CH3:24])[NH:20][C:8]=3[C:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)=[CH:12][CH:11]=2)[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 612Lactic AcidHCID 226422693,6-Diphenyl-1,2-benzenediamine

생성물 1

HCID 21107906HCID 21107906, 화합물수율 82.8%

반응 조건

온도
140 °C

실험 절차

A mixture of 1.25 g (4.8 mmol) 1,1′:4′,1″-terphenyl-2′,3′-diamine, 0.75 ml (8.6 mmol) 85% aq. lactic acid and 4.8 ml 4N HCl were stirred at reflux for 6 hours and then the volatile materials evaporated over 1 hour. The oily residue was heated to 140° C. and stirred for 15 min. After cooling to room temperature 10 ml water were added and the mixture triturated for 30 min. Addition of conc. NH4OH to pH˜7.5–8 followed by filtration, washing with water (4×10 ml) and drying under vacuum at 60° C. gave 1.25 g (82.8%) of the desired product. 1H NMR (250 MHz, CDCl3), δ, ppm: 1.58 (d, JHH=6.7 Hz, 3H), 3.64 (br.s, 1H), 5.07 (q, 1H), 7.37–7.76 (m, 12 H), 9.53 (br. s, 1H).

후처리

  1. temperatureat reflux for 6 hours
  2. customthe volatile materials evaporated over 1 hour
  3. stirringstirred for 15 min
  4. temperatureAfter cooling to room temperature 10 ml water
  5. additionwere added
  6. customthe mixture triturated for 30 min
  7. additionAddition of conc. NH4OH to pH˜7.5–8
  8. filtrationfollowed by filtration
  9. washwashing with water (4×10 ml)
  10. customdrying under vacuum at 60° C.

출처 및 근거

ORD 기록
ord-76c37df206514dbaa5dd3d8a53a66a9f
출처 데이터셋
uspto-grants-2007_06
특허 번호
US07229943B2

반응 노트

불러오는 중…