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Toluene → HCID 21442848, 화합물

HRID 1606511
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HRID 1606511 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][OH:16])[CH2:10][CH2:9]2)[CH:5]=[CH:6][CH:7]=1.[C:17]12[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=1)[NH:22]C(=O)O[C:18]2=[O:19].C1(C)C=CC=CC=1>CCOCC>[C:18]([O:16][CH2:15][CH2:14][N:11]1[CH2:10][CH2:9][N:8]([C:4]2[CH:5]=[CH:6][CH:7]=[C:2]([Cl:1])[CH:3]=2)[CH2:13][CH2:12]1)(=[O:19])[C:17]1[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=1)[NH2:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1140TolueneHCID 8359Isatoic AnhydrideHCID 967031-Piperazineethanol, 4-(3-chlorophenyl)-

생성물 1

HCID 21442848HCID 21442848, 화합물수율 70%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

7.2 G. (0.03 mol) of 2-(4-m-chlorophenyl-piperazino)-ethanol and 6.55 g. (0.04 mol) of isatoic anhydride in 125 ml. of toluene are refluxed for 3 hours. The hot toluene solution is filtered and the toluene is evaporated from the filtrate to give a residue which is taken up in ether in order to remove a small amount of unreacted isatoic anhydride, the solution is filtered and the ether is driven off. The remaining product is triturated in petroleum ether, filtered off and recrystallised twice from isopropyl alcohol to give 7.6 g. (yield = 70%) of 2-(4-m-chlorophenylpiperazino)-ethyl anthranilate, which melts at 76°C.

후처리

  1. filtrationThe hot toluene solution is filtered
  2. customthe toluene is evaporated from the filtrate
  3. customto give a residue which
  4. customto remove a small amount of unreacted isatoic anhydride
  5. filtrationthe solution is filtered
  6. customThe remaining product is triturated in petroleum ether
  7. filtrationfiltered off
  8. customrecrystallised twice from isopropyl alcohol
  9. customto give 7.6 g

출처 및 근거

ORD 기록
ord-3b06104217764322b5bb29aebb5a013c
출처 데이터셋
uspto-grants-1976_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03953449

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