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Sodium Iodide → HCID 86748649, 화합물

HRID 1655015
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HRID 1655015 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]2[CH2:16][CH2:15][NH:14][CH2:13][CH:12]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].O[C:18]1(C2C=CC(OC)=C(OC)C=2)C[CH2:22][NH:21][CH2:20][CH2:19]1.C1(C)C=CC(S(O)(=O)=[O:41])=CC=1.ClCCCNC([N:52]1[CH2:56][CH2:55][CH2:54][C:53]1=[O:57])=O.C([O-])([O-])=O.[K+].[K+].[Na+].[I-]>CN(C=O)C.C(OCC)(=O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]2[CH2:16][CH2:15][N:14]([N:21]([CH2:20][CH2:19][CH3:18])[C:22]([CH:54]3[CH2:55][CH2:56][NH:52][C:53]3=[O:57])=[O:41])[CH2:13][CH:12]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 6

HCID 5238Sodium IodideHCID 6101p-Toluenesulfonic acidHCID 11430Potassium CarbonateHCID 6129904-(3,4-Dimethoxyphenyl)-1,2,3,6-tetrahydropyridineHCID 14441092HCID 14441092, 화합물HCID 150347144-(3,4-Dimethoxyphenyl)piperidin-4-ol

생성물 1

HCID 86748649
HCID 86748649, 화합물
수율 33.4%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 3.76 g of 4-(3,4-dimethoxyphenyl)-1,2,5, 6-tetrahydropyridine (V-7), which was prepared by the reaction of 4-hydroxy-4-(3,4-dimethoxyphenyl)piperidine and p-toluenesulfonic acid, and 2.94 g of 1-(3-chloropropylcarbamoyl)-2-oxopyrrolidine in 35 ml of DMF is added 3.98 g of K2CO3 and 3.22 g of NaI. The reaction mixture is stirred at 100°-105° C. for 6 days under nitrogen gas. After cooling to room temperature, the mixture is diluted with ethyl acetate, washed with brine and dried over MgSO4. After removal of the solvent, the residue is subjected to column chromatography with silica gel, eluting with CH2Cl2 /MeOH (20/1) to prepare 1.78 g (Yield: 33.4%) of the compound (I a-105) as solid. The oxalate is recrystallized from iPrOH-MeOH to prepare needles. mp. 178.0°-182.0° C.

후처리

  1. washwashed with brine
  2. dry with materialdried over MgSO4
  3. customAfter removal of the solvent
  4. washeluting with CH2Cl2 /MeOH (20/1)

출처 및 근거

ORD 기록
ord-8454f2b4333948a2ab8b49bae6994e04
출처 데이터셋
uspto-grants-1995_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05410058

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