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Trifluoroacetic acid → HCID 66603393, 화합물

HRID 403550
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HRID 403550 반응식
[CH2:1]([O:8][C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[N:15]([CH:19]1[CH2:24][CH2:23][N:22](C(OC(C)(C)C)=O)[CH2:21][CH2:20]1)[C:14](=[O:32])[N:13]([CH2:33][C:34]1[CH:39]=[CH:38][C:37]([O:40][CH3:41])=[C:36]([O:42][CH3:43])[CH:35]=1)[C:12]2=[O:44])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(O)(C(F)(F)F)=O.C([O-])([O-])=O.[K+].[K+]>C(Cl)Cl>[CH2:1]([O:8][C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[N:15]([CH:19]1[CH2:20][CH2:21][NH:22][CH2:23][CH2:24]1)[C:14](=[O:32])[N:13]([CH2:33][C:34]1[CH:39]=[CH:38][C:37]([O:40][CH3:41])=[C:36]([O:42][CH3:43])[CH:35]=1)[C:12]2=[O:44])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 11430Potassium CarbonateHCID 595870451,1-Dimethylethyl 4-[6-(benzyloxy)-3-(3,4-dimethoxybenzyl)-2,4-dioxo-3,4-dihydroquinazolin-1(2H)-yl]piperidine-1-carboxylate

생성물 1

HCID 66603393HCID 66603393, 화합물수율 91.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of 3.5 g of 1,1-dimethylethyl 4-[6-(benzyloxy)-3-(3,4-dimethoxybenzyl)-2,4-dioxo-3,4-dihydroquinazolin-1(2H)-yl]piperidine-1-carboxylate obtained in stage 1.5 and 25 ml of TFA in 50 ml of DCM is stirred at AT for 2 h 00. The mixture is neutralized with K2CO3. It is filtered and the filtrate is evaporated under reduced pressure. The residue is taken up in DCM and washed with a saturated NaHCO3 solution and then with an 8% NaOH solution. The solution is dried over Na2SO4 and filtered, and the solvent is evaporated under reduced pressure to give 2.67 g of the expected product.

후처리

  1. filtrationIt is filtered
  2. customthe filtrate is evaporated under reduced pressure
  3. washwashed with a saturated NaHCO3 solution
  4. dry with materialThe solution is dried over Na2SO4
  5. filtrationfiltered
  6. customthe solvent is evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-2e9c6cdae32a448189bf5a430f42b2a2
출처 데이터셋
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08748441B2

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