3-Aminophenyl dimethylcarbamate → HCID 67036855, 화합물

HRID 216074노트

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HRID 216074 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][C:11]([CH2:17][CH2:18][N:19]([CH3:21])[CH3:20])([C:14](O)=[O:15])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.C(N(CC)C(C)C)(C)C.[CH3:55][N:56]([CH3:67])[C:57](=[O:66])[O:58][C:59]1[CH:64]=[CH:63][CH:62]=[C:61]([NH2:65])[CH:60]=1>C(OC(C)C)(=O)C.CCOC(C)=O>[CH3:20][N:19]([CH3:21])[CH2:18][CH2:17][C:11]1([C:14](=[O:15])[NH:65][C:61]2[CH:62]=[CH:63][CH:64]=[C:59]([O:58][C:57](=[O:66])[N:56]([CH3:55])[CH3:67])[CH:60]=2)[CH2:10][CH2:9][N:8]([C:6]([O:5][C:1]([CH3:2])([CH3:3])[CH3:4])=[O:7])[CH2:13][CH2:12]1

참가 물질

7

반응물 4

HCID 298773-Aminophenyl dimethylcarbamateHCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 670368571-(Tert-butoxycarbonyl)-4-(2-(dimethylamino)ethyl)piperidine-4-carboxylic acid

생성물 1

HCID 67036855HCID 67036855, 화합물

시약·촉매·용매 2

HCID 7915Isopropyl Acetate용매HCID 8857Ethyl Acetate용매

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온도
85 °C

실험 절차

1-(tert-Butoxycarbonyl)-4-(2-(dimethylamino)ethyl)piperidine-4-carboxylic acid from step B (100 mg, 0.33 mmol), HATU (175 mg, 0.46 mmol), and N,N-diisopropylethylamine (0.116 mL, 0.67 mmol) were stirred in isopropyl acetate for 10 minutes. 3-aminophenyl dimethylcarbamate (90 mg, 0.5 mmol) was added, and the reaction was stirred at 85° C. for 2 hours, cooled to room temperature, stirred overnight, and then diluted with EtOAc, washed with sat. aq. Na2CO3 and brine (with back extraction), dried over MgSO4, filtered, and concentrated under vacuum, to give the title compound as a viscous oil. MS (ES+) [M+H]+=463.

후처리

  1. temperaturecooled to room temperature
  2. stirringstirred overnight
  3. washwashed with sat. aq. Na2CO3 and brine (with back extraction)
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-be9ba0704e534dcb843e516760891a53
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08193202B2

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