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Trifluoroacetic acid → HCID 178473785, 화합물

HRID 1488050
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HRID 1488050 반응식
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([CH:9]2[CH2:12][N:11]([C:13]([C:15]3[CH:16]=[CH:17][C:18]([CH3:40])=[C:19]([C:21]4[N:22]=[C:23]([CH:27]5[CH2:32][CH2:31][N:30]([C:33]([O:35]C(C)(C)C)=O)[CH2:29][CH2:28]5)[NH:24][C:25]=4[CH3:26])[CH:20]=3)=[O:14])[CH2:10]2)=[CH:5][CH:4]=1)#[N:2].F[C:42](F)(F)C(O)=O.CC1C=CC(C(N2CC(C3C=CC(C#N)=CC=3)C2)=O)=CC=1C1NC(C2CCNCC2)=NC=1C.C(OC(=O)C)(=O)C.C(N(CC)CC)C>C(Cl)Cl>[C:33]([N:30]1[CH2:31][CH2:32][CH:27]([C:23]2[NH:22][C:21]([C:19]3[CH:20]=[C:15]([CH:16]=[CH:17][C:18]=3[CH3:40])[C:13]([N:11]3[CH2:10][CH:9]([C:6]4[CH:5]=[CH:4][C:3]([C:1]#[N:2])=[CH:8][CH:7]=4)[CH2:12]3)=[O:14])=[C:25]([CH3:26])[N:24]=2)[CH2:28][CH2:29]1)(=[O:35])[CH3:42]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 6422Trifluoroacetic acidHCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 90021783t-Butyl 4-(4-(5-(3-(4-cyanophenyl)azetidine-1-carbonyl)-2-methylphenyl)-5-methyl-1H-imidazol-2-yl)piperidine-1-carboxylate2회HCID 178425785HCID 178425785, 화합물

생성물 1

HCID 178473785
HCID 178473785, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of tert-butyl 4-(4-(5-(3-(4-cyanophenyl)azetidine-1-carbonyl)-2-methylphenyl)-5-methyl-1H-imidazol-2-yl)piperidine-1-carboxylate (compound 182.3, 475 mg, 0.88 mmol) in 20 mL DCM, was added trifluoroacetic acid (4 mL). The reaction was stirred for 1.5 hours, concentrated under reduced pressure and neutralized with 10 mL Na2CO3 (1M) to obtain a crude product after lyophilization. A mixture of 4-(1-(4-methyl-3-(4-methyl-2-(piperidin-4-yl)-1H-imidazol-5-yl)benzoyl)azetidin-3-yl)benzonitrile (252 mg, 0.57 mmol), acetic anhydride (71 μL, 0.75 mmol) and triethylamine (120 μL, 0.86 mmol) was stirred at room temperature for 16 hours. The reaction was concentrated under reduced pressure, then diluted with saturated NaH2PO4 (20 mL) and extracted with EtOAc (3×20 mL). The organic phase was dried over MgSO4 and concentrated under reduced pressure. The residue was purified by preparative TLC with 10% methanol in dichloromethane and lyophilized to give 235 mg (80%-2 steps) of the title compound as a white solid. m/z (ES+) 482 (M+H)+.

후처리

  1. concentrationconcentrated under reduced pressure and neutralized with 10 mL Na2CO3 (1M)
  2. customto obtain a crude product after lyophilization
  3. stirringwas stirred at room temperature for 16 hours
  4. concentrationThe reaction was concentrated under reduced pressure
  5. additiondiluted with saturated NaH2PO4 (20 mL)
  6. extractionextracted with EtOAc (3×20 mL)
  7. dry with materialThe organic phase was dried over MgSO4
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was purified by preparative TLC with 10% methanol in dichloromethane

출처 및 근거

ORD 기록
ord-8e8be8e10c464878b0dad1b67a5dc8c9
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09428502B2

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