Sodium Chloride → [(E)-1-aminoethylideneamino] 6-[(5-cyanopyrazin-2-yl)amino]-4-[[1-[(2-methylpropan-2-yl)oxycarbonyl]piperidin-4-yl]methylamino]pyridine-3-carboxylate

HRID 384671ノート

反応式

HRID 384671 の反応式
CCN(C(C)C)C(C)C.[C:10]([O:14][C:15]([N:17]1[CH2:22][CH2:21][CH:20]([CH2:23][NH:24][C:25]2[C:30]([C:31]([OH:33])=[O:32])=[CH:29][N:28]=[C:27]([NH:34][C:35]3[CH:40]=[N:39][C:38]([C:41]#[N:42])=[CH:37][N:36]=3)[CH:26]=2)[CH2:19][CH2:18]1)=[O:16])([CH3:13])([CH3:12])[CH3:11].CN(C(O[N:51]1N=N[C:53]2C=CC=[N:57][C:52]1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.O/N=C(/N)\C.[Na+].[Cl-]>CN(C=O)C>[NH2:57]/[C:52](=[N:51]/[O:32][C:31]([C:30]1[C:25]([NH:24][CH2:23][CH:20]2[CH2:19][CH2:18][N:17]([C:15]([O:14][C:10]([CH3:13])([CH3:11])[CH3:12])=[O:16])[CH2:22][CH2:21]2)=[CH:26][C:27]([NH:34][C:35]2[CH:40]=[N:39][C:38]([C:41]#[N:42])=[CH:37][N:36]=2)=[N:28][CH:29]=1)=[O:33])/[CH3:53]

参加物

7

反応物 5

HCID 5234Sodium ChlorideHCID 81531DiisopropylethylamineHCID 5360664N-HydroxyacetamidineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 596134654-((1-(Tert-butoxycarbonyl)piperidin-4-yl)methylamino)-6-(5-cyanopyrazin-2-ylamino)nicotinic acid

生成物 1

HCID 59613429[(E)-1-aminoethylideneamino] 6-[(5-cyanopyrazin-2-yl)amino]-4-[[1-[(2-methylpropan-2-yl)oxycarbonyl]piperidin-4-yl]methylamino]pyridine-3-carboxylate収率 77%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

DIPEA (96 μL, 0.55 mmol) was added to a solution of 4-((1-(tert-butoxycarbonyl)piperidin-4-yl)methylamino)-6-(5-cyanopyrazin-2-ylamino)nicotinic acid (Synthesis 75-A) (50 mg, 0.11 mmol), HATU (54 mg, 0.14 mmol) in DMF (6 mL) under argon. The reaction mixture was stirred for 15 min at r.t. and (E)-N′-hydroxyacetimidamide (25 mg, 0.34 mmol) in DMF (0.5 mL) was added. The resulting solution was stirred at r.t. for 12 hr. Aqueous NaCl solution (15 mL) was added and the resulting precipitate was collected. The solid was washed with water and n-hexane to give a yellow powder (43 mg, 77%).

後処理

  1. stirringThe resulting solution was stirred at r.t. for 12 hr
  2. customthe resulting precipitate was collected
  3. washThe solid was washed with water and n-hexane

出典と根拠

ORDレコード
ord-3b5f3b6745004473a25c317baf6eb4fe
出典データセット
uspto-grants-2013_02
特許番号
US08367658B2

反応ノート

読み込み中…