Diisopropylethylamine → Nvp-tnks-656

HRID 713477ノート

反応式

HRID 713477 の反応式
[CH3:1][O:2][C:3]1[CH:20]=[CH:19][C:6]([C:7]([CH:9]2[CH2:14][CH2:13][N:12]([CH2:15][C:16]([OH:18])=O)[CH2:11][CH2:10]2)=[O:8])=[CH:5][CH:4]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C.[CH:54]1([CH2:57][NH:58][CH2:59][C:60]2[NH:61][C:62](=[O:70])[C:63]3[CH2:69][O:68][CH2:67][CH2:66][C:64]=3[N:65]=2)[CH2:56][CH2:55]1>CN(C=O)C>[CH:54]1([CH2:57][N:58]([CH2:59][C:60]2[NH:61][C:62](=[O:70])[C:63]3[CH2:69][O:68][CH2:67][CH2:66][C:64]=3[N:65]=2)[C:16](=[O:18])[CH2:15][N:12]2[CH2:11][CH2:10][CH:9]([C:7](=[O:8])[C:6]3[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[CH:20][CH:19]=3)[CH2:14][CH2:13]2)[CH2:56][CH2:55]1

参加物

6

反応物 4

HCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 712267662-(4-(4-Methoxybenzoyl)piperidin-1-YL)acetic acidHCID 1362440742-[(Cyclopropylmethyl-amino)-methyl]-3,5,7,8-tetrahydro-pyrano[4,3-d]pyrimidin-4-one

生成物 1

HCID 136237316Nvp-tnks-656収率 22.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

To [4-(4-methoxy-benzoyl)-piperidin-1-yl]-acetic acid (306 mg, 0.85 mmol) in DMF (3 mL) was added with HATU (485 mg, 1.28 mmol) and DIEA (0.37 mL, 275 mg, 2.12 mmol). This was sonicated, stirred for 30 min and then 2-[(cyclopropylmethyl-amino)-methyl]-3,5,7,8-tetrahydro-pyrano[4,3-d]pyrimidin-4-one (200 mg, 0.85 mmol) in 1 mL DMF was added to the mixture. Then it was stirred at room temperature for 16 hours and the mixture was concentrated to dryness. This was purified by silica gel column (eluted with 0-10% methanol in dichloromethane) followed by trituration with methanol to give a white solid as the title compound (93 mg, 0.19 mmol, 22% yield). m/z=495.3 (M+H).

後処理

  1. customThis was sonicated
  2. stirringThen it was stirred at room temperature for 16 hours
  3. concentrationthe mixture was concentrated to dryness
  4. customThis was purified by silica gel column (eluted with 0-10% methanol in dichloromethane)

出典と根拠

ORDレコード
ord-02d37089e0574c2eaf49127320b06ded
出典データセット
uspto-grants-2015_11
特許番号
US09181266B2

反応ノート

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