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Acetic Acid → HCID 59239087, 화합물

HRID 1698023
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HRID 1698023 반응식
[CH2:1]([NH:3][C:4]([NH:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[N:14]=[C:15]([N:26]3[CH2:31][CH2:30][O:29][CH2:28][C@@H:27]3[CH3:32])[C:16]3[CH2:22][CH2:21][N:20]([CH2:23][CH3:24])[C@@H:19]([CH3:25])[C:17]=3[N:18]=2)=[CH:9][CH:8]=1)=[O:5])[CH3:2].C(NC(NC1C=CC(C2N=C(N3CCOC[C@@H]3C)C3CCNC(C)C=3N=2)=CC=1)=O)C.CN(C)C=O.C(=O)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(O)(=O)C>[OH-].[Na+]>[CH2:1]([NH:3][C:4]([NH:6][C:7]1[CH:8]=[CH:9][C:10]([C:13]2[N:14]=[C:15]([N:26]3[CH2:31][CH2:30][O:29][CH2:28][C@@H:27]3[CH3:32])[C:16]3[CH2:22][CH2:21][N:20]([CH2:23][CH3:24])[C@H:19]([CH3:25])[C:17]=3[N:18]=2)=[CH:11][CH:12]=1)=[O:5])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 6

HCID 176Acetic Acid2회HCID 177Acetaldehyde2회HCID 6228Dimethylformamide2회HCID 5049666Sodium triacetoxyborohydride2회HCID 592396421-ethyl-3-(4-((S)-7-ethyl-8-methyl-4-((S)-3-methylmorpholino)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-2-yl)phenyl)ureaHCID 67178079HCID 67178079, 화합물

생성물 1

HCID 59239087HCID 59239087, 화합물

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매2회

실험 절차

and 1-ethyl-3-(4-((S)-7-ethyl-8-methyl-4-((S)-3-methylmorpholino)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-2-yl)phenyl)urea (ws2): (1-Ethyl-3-(4-(8-methyl-4-((S)-3-methylmorpholino)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-2-yl)phenyl)urea (0.172 g, 0.419 mmol) in dry N,N-Dimethylformamide (2.00 mL, 25.8 mmol) at 0° C. was added Acetaldehyde (0.0236 mL, 0.420 mmol). The reaction mixture was stirred at 0° C. for 5 minutes the added Sodium triacetoxyborohydride (0.182 g, 0.859 mmol) followed by Acetic acid (0.0476 mL, 0.838 mmol). The reaction mixture was allowed to warm slowly to room temperature and stirred overnight. The reaction mixture was diluted with 1 M NaOH, extracted three times with 10% MeOH in dichloromethane, dried over Magnesium sulfate, filtered, and concentrated. The reaction mixture was redissovled in dry N,N-Dimethylformamide (2.00 mL, 25.8 mmol) cooled at 0° C., then added Acetaldehyde (0.0236 mL, 0.420 mmol). The reaction mixture was stirred at 0° C. for 5 minutes then added Sodium triacetoxyborohydride (0.181 g, 0.854 mmol) followed by Acetic acid (0.0476 mL, 0.837 mmol). The reaction mixture was stirred for 3 days. The reaction mixture was diluted with 1M NaOH, extracted three times with 10% MeOH in dichloromethane, dried over Magnesium sulfate, filtered, concentrated, purified by HPLC, and the diastereomers were separated by SFC. R Diastereomer (ws1): 1H NMR (400 MHz, DMSO) δ 8.66 (s, 1H), 8.17 (d, J=8.7, 2H), 7.47 (d, J=8.8, 2H), 6.19 (t, J=5.6, 1H), 4.12 (d, J=6.7, 1H), 3.87 (d, J=11.1, 1H), 3.73 (dd, J=11.3, 2.7, 1H), 3.64-3.49 (m, 4H), 3.47-3.38 (m, 2H), 3.16-3.09 (m, 2H), 3.01-2.93 (m, 1H), 2.80 (dq, J=14.5, 7.3, 1H), 2.67 (t, J=7.4, 1H), 2.60-2.53 (m, 1H), 2.41-2.31 (m, 1H), 1.42 (d, J=6.6, 3H), 1.18 (d, J=6.6, 3H), 1.14 (t, J=7.2, 3H), 1.06 (t, 3H). LC/MS-m/z+439.3 (M+H)+; and S-Diastereomer (ws2): 1H NMR (400 MHz, DMSO) δ 8.65 (s, 1H), 8.17 (d, J=8.7, 2H), 7.47 (d, J=8.8, 2H), 6.19 (t, J=5.5, 1H), 4.08 (d, J=6.7, 1H), 3.86 (d, J=11.3, 1H), 3.71-3.55 (m, 5H), 3.39 (d, J=11.4, 1H), 3.16-3.08 (m, 2H), 2.90 (dd, J=11.6, 4.7, 1H), 2.74 (dq, J=14.3, 7.2, 1H), 2.69-2.53 (m, 3H), 2.47-2.40 (m, 1H), 1.38 (d, J=6.6, 3H), 1.29 (d, J=6.6, 3H), 1.13 (t, J=7.2, 3H), 1.07 (t, 3H).

후처리

  1. extractionextracted three times with 10% MeOH in dichloromethane
  2. dry with materialdried over Magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. temperaturecooled at 0° C.
  6. stirringThe reaction mixture was stirred at 0° C. for 5 minutes
  7. stirringThe reaction mixture was stirred for 3 days
  8. extractionextracted three times with 10% MeOH in dichloromethane
  9. dry with materialdried over Magnesium sulfate
  10. filtrationfiltered
  11. concentrationconcentrated
  12. custompurified by HPLC
  13. customthe diastereomers were separated by SFC

출처 및 근거

ORD 기록
ord-50ca67edf05148efb87241b8a80cd5a8
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08163763B2

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