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Piperazine → HCID 18186793, 화합물

HRID 1296671
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HRID 1296671 반응식
Cl[C:2]1[CH:7]=[N:6][CH:5]=[C:4]([O:8][CH2:9][CH2:10][O:11][C:12]2[CH:21]=[CH:20][C:19]3[C:14](=[CH:15][CH:16]=[C:17]([O:22][CH3:23])[CH:18]=3)[CH:13]=2)[N:3]=1.[CH3:24][O:25][C:26]1[CH:27]=[C:28]2[C:33](=[CH:34][CH:35]=1)[CH:32]=[C:31]([O:36][CH2:37][CH2:38][OH:39])[CH:30]=[CH:29]2.[NH:40]1[CH2:45][CH2:44][NH:43][CH2:42][CH2:41]1.C([O-])([O-])=O.[K+].[K+].COC1C=C2C(=CC=1)C=C(O)C=C2.C1(=O)OCCO1>CO.C(Cl)(Cl)Cl.CCCCCC>[CH3:23][O:22][C:17]1[CH:18]=[C:19]2[C:14](=[CH:15][CH:16]=1)[CH:13]=[C:12]([O:11][CH2:10][CH2:9][O:8][C:4]1[CH:5]=[N:6][CH:7]=[C:2]([N:40]3[CH2:45][CH2:44][NH:43][CH2:42][CH2:41]3)[N:3]=1)[CH:21]=[CH:20]2.[CH3:24][O:25][C:26]1[CH:27]=[C:28]2[C:33](=[CH:34][CH:35]=1)[CH:32]=[C:31]([O:36][CH2:37][CH2:38][OH:39])[CH:30]=[CH:29]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 6

HCID 4837PiperazineHCID 7303Ethylene carbonateHCID 11430Potassium CarbonateHCID 2886346-Methoxy-2-naphtholHCID 18186793HCID 18186793, 화합물HCID 18186892HCID 18186892, 화합물

생성물 2

HCID 18186793HCID 18186793, 화합물
HCID 18186912HCID 18186912, 화합물

시약·촉매·용매 1

HCID 22285155HCID 22285155, 화합물용매

실험 절차

The title compound was prepared according to the procedure of example 50, step 2, starting from 2-chloro-6-[2-(6-methoxy-naphthalen-2-yloxy)-ethoxy]pyrazine [0.94 g, 2.8 mmol; obtained according to the procedure of example 50, step 1, starting from 2-(6-methoxy-naphthalen-2-yloxy)ethanol*], piperazine (1.00 g, 11.6 mmol) and K2CO3 (0.50 g, 3.6 mmol) with the exception that the final filtration through alumina was omitted. The yield of the of the title compound was 0.52 g (48%) which was obtained as a beige colored solid. Purity 100% (HPLC). MS m/z 380 (M)+. HRMS m/z calcd for C21H24N4O3 (M)+ 380.1848, found 380.1845. *Prepared from 6-methoxy-2-naphthol and ethylene carbonat according to the procedure of Example 134, step 1, in WO 00/76984. The reaction mixture was refluxed for 2 h. Pure 2-(6-methoxy-naphthalen-2-yloxy)ethanol was obtained by recrystallization from MeOH/CHCl3/n-hexane.

후처리

  1. customobtained
  2. filtrationfiltration through alumina
  3. customwas obtained as a beige colored solid
  4. temperatureThe reaction mixture was refluxed for 2 h

출처 및 근거

ORD 기록
ord-2225d59e48f34390a1740d04b5ebec30
출처 데이터셋
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07247633B2

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