Diisopropylethylamine → HCID 66823460、化合物

HRID 1909998ノート

反応式

HRID 1909998 の反応式
Cl.Cl.[NH:3]1[C:11]2[C:6](=[CH:7][C:8]([C:12]3[C:20]4[C:15](=[N:16][CH:17]=[N:18][C:19]=4[NH2:21])[N:14]([CH3:22])[N:13]=3)=[CH:9][CH:10]=2)[CH2:5][CH2:4]1.[Cl:23][C:24]1[C:25]([F:34])=[C:26]([CH2:30][C:31](O)=[O:32])[CH:27]=[CH:28][CH:29]=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>CN(C=O)C.O>[Cl:23][C:24]1[C:25]([F:34])=[C:26]([CH2:30][C:31]([N:3]2[C:11]3[C:6](=[CH:7][C:8]([C:12]4[C:20]5[C:15](=[N:16][CH:17]=[N:18][C:19]=5[NH2:21])[N:14]([CH3:22])[N:13]=4)=[CH:9][CH:10]=3)[CH2:5][CH2:4]2)=[O:32])[CH:27]=[CH:28][CH:29]=1

参加物

7

反応物 4

HCID 81531DiisopropylethylamineHCID 27737203-Chloro-2-fluorophenylacetic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 668235503(2,3-dihydro-1H-indol-5-yl)-1-methyl-1H-pyrazolo[3,4-d]pyrimidin-4-amine 2HCl

生成物 1

HCID 66823460HCID 66823460、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

In a 20 mL vial with cap, to the solution of 3-(2,3-dihydro-1H-indol-5-yl)-1-methyl-1H-pyrazolo[3,4-d]pyrimidin-4-amine 2HCl (65.3 mg, 0.192 mmol), (3-chloro-2-fluorophenyl)acetic acid (36.3 mg, 0.192 mmol), HATU (73.2 mg, 0.192 mmol) in DMF (2 mL) was added Hunig's base (0.134 mL, 0.770 mmol). The mixture was stirred overnight. The reaction was poured into water, and off-white solid formed. The solid was filtered to give the title compound as an off-white solid. It has 0.75 eq. of DMF based on NMR. 1H NMR (400 MHz, DMSO-d6) δ ppm 3.25-3.31 (m, 2H), 3.94 (s, 3H), 4.04 (s, 2H), 4.32 (t, J=8.46 Hz, 2H), 7.20-7.26 (m, 1H), 7.33 (d, J=1.52 Hz, 1H), 7.35 (s, 1H), 7.44 (d, J=8.08 Hz, 1H), 7.50-7.57 (m, 2H), 8.14 (d, J=8.34 Hz, 1H), 8.25 (s, 1H).

後処理

  1. customformed
  2. filtrationThe solid was filtered

出典と根拠

ORDレコード
ord-e4851f510fff45448238525d501648ee
出典データセット
uspto-grants-2013_12
特許番号
US08598156B2

反応ノート

読み込み中…