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Hydrochloric Acid → HCID 14556333, 화합물

HRID 1087747
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HRID 1087747 반응식
[C:1]([C:5]1[CH:15]=[CH:14][C:8]2[N:9]([CH3:13])[C:10](=[O:12])[O:11][C:7]=2[CH:6]=1)(=[O:4])[CH2:2][CH3:3].[F:16][C:17]([F:31])([F:30])[C:18]1[CH:19]=[C:20]([N:24]2[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]2)[CH:21]=[CH:22][CH:23]=1.Cl.[CH2:33](O)CC>>[CH3:13][N:9]1[C:8]2[CH:14]=[CH:15][C:5]([C:1](=[O:4])[CH:2]([CH3:33])[CH2:3][N:27]3[CH2:28][CH2:29][N:24]([C:20]4[CH:21]=[CH:22][CH:23]=[C:18]([C:17]([F:16])([F:30])[F:31])[CH:19]=4)[CH2:25][CH2:26]3)=[CH:6][C:7]=2[O:11][C:10]1=[O:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 313Hydrochloric AcidHCID 10311-PropanolHCID 42961-(3-(Trifluoromethyl)phenyl)piperazineHCID 3043000JPB 5

생성물 1

HCID 14556333HCID 14556333, 화합물

실험 절차

0.025 mole of 6-propionyl-3-methylbenzoxazolinone, described in French Patent No. 73/23,280, and 0.038 mole of 1-(3-trifluoromethylphenyl)piperazine are dissolved in 150 cm3 of propanol in a 250-cm3 groundnecked flask equipped with a reflux condenser and a magnetic stirrer. 0.038 mole of trioxymethylene and 1.5 cm3 of concentrated hydrochloric acid are added. The mixture is heated to reflux for 72 hours. The precipitate formed is drained, washed with acetone, suspended in water and alkalinized with sodium hydroxide. The mixture is extracted several times with chloroform, the organic phases are combined, dried over calcium chloride, filtered and evaporated on a water bath under vacuum and the residue is recrystallized in propanol.

후처리

  1. customequipped with a reflux condenser and a magnetic stirrer
  2. temperatureThe mixture is heated
  3. temperatureto reflux for 72 hours
  4. customThe precipitate formed
  5. washwashed with acetone
  6. extractionThe mixture is extracted several times with chloroform
  7. dry with materialdried over calcium chloride
  8. filtrationfiltered
  9. customevaporated on a water bath under vacuum
  10. customthe residue is recrystallized in propanol

출처 및 근거

ORD 기록
ord-6d8bbbd1d77f45edbfc6a8186c2b44ac
출처 데이터셋
uspto-grants-1990_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04960778

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