Diisopropylethylamine → HCID 58117637、化合物

HRID 405944

反応式

HRID 405944 の反応式
[O:1]=[S:2]1[C:10]2[C:9]([NH:11][CH:12]3[CH2:17][CH2:16][O:15][CH2:14][CH2:13]3)=[N:8][C:7]([N:18]3[CH2:23][CH2:22][CH:21]([C:24]4[CH:25]=[C:26]([CH:30]=[CH:31][CH:32]=4)[C:27](O)=[O:28])[CH2:20][CH2:19]3)=[N:6][C:5]=2[CH2:4][CH2:3]1.C([N:36]([CH:39]([CH3:41])[CH3:40])[CH2:37]C)(C)C.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.Cl.C1(CN)CC1>CN(C)C=O>[CH:39]1([N:36]([CH3:37])[C:27](=[O:28])[C:26]2[CH:30]=[CH:31][CH:32]=[C:24]([CH:21]3[CH2:20][CH2:19][N:18]([C:7]4[N:8]=[C:9]([NH:11][CH:12]5[CH2:17][CH2:16][O:15][CH2:14][CH2:13]5)[C:10]5[S:2](=[O:1])[CH2:3][CH2:4][C:5]=5[N:6]=4)[CH2:23][CH2:22]3)[CH:25]=2)[CH2:40][CH2:41]1

参加物

6

反応物 4

HCID 81531DiisopropylethylamineHCID 81671(Cyclopropylmethyl)ammonium chlorideHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 58117546HCID 58117546、化合物

生成物 1

HCID 58117637HCID 58117637、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

59.8 mg 3-{1-[5-oxo-4-(tetrahydropyran-4-ylamino)-6,7-dihydro-5H-5λ4-thieno[3,2-d]pyrimidin-2-yl]-piperidin-4-yl}-benzoic acid are placed in 2.3 ml dimethylformamide, then 91 l diisopropylethylamine and 60 mg O-(7-azabenzotriazol-1-yl-)-N,N,N′,N′-tetramethyluronium hexafluorophosphate (HATU) are added. After 15 min a mixture of 15.5 mg cyclopropylmethylamine hydrochloride in 300 l dimethylformamide is added. The reaction mixture is stirred at ambient temperature until there is no further reaction, and the product is purified directly by preparative HPLC (method B). 50 mg Example 249 are obtained as a solid. Analytical HPLC-MS (method D): RT=1.05 min.

後処理

  1. additionis added
  2. customno further reaction
  3. customthe product is purified directly by preparative HPLC (method B)

出典と根拠

ORDレコード
ord-fcb79a69383b461ba1f1519ec6a1cf14
出典データセット
uspto-grants-2014_06
特許番号
US08754073B2

関連ノート

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