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Acetic Acid → HCID 59239087、化合物

HRID 1698023
ノート
印刷プレビュー

反応式

HRID 1698023 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 6

HCID 176Acetic Acid2 回HCID 177Acetaldehyde2 回HCID 6228Dimethylformamide2 回HCID 5049666Sodium triacetoxyborohydride2 回HCID 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、化合物

生成物 1

HCID 59239087HCID 59239087、化合物

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-50ca67edf05148efb87241b8a80cd5a8
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08163763B2

反応ノート

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