Diisopropylethylamine → HCID 58447638、化合物

HRID 1036299ノート

反応式

HRID 1036299 の反応式
[S:1]1[CH2:6][CH2:5][N:4]([C:7]2[N:12]=[CH:11][C:10]([CH2:13][C:14]([OH:16])=O)=[CH:9][CH:8]=2)[CH2:3][CH2:2]1.[F:17][C:18]1[CH:19]=[C:20]([C:24]2[N:29]=[CH:28][C:27]([NH2:30])=[CH:26][CH:25]=2)[CH:21]=[CH:22][CH:23]=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.C(OCC)(=O)C.O>[F:17][C:18]1[CH:19]=[C:20]([C:24]2[N:29]=[CH:28][C:27]([NH:30][C:14](=[O:16])[CH2:13][C:10]3[CH:11]=[N:12][C:7]([N:4]4[CH2:3][CH2:2][S:1][CH2:6][CH2:5]4)=[CH:8][CH:9]=3)=[CH:26][CH:25]=2)[CH:21]=[CH:22][CH:23]=1

参加物

8

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 463118956-(3-Fluorophenyl)pyridin-3-amineHCID 58447828HCID 58447828、化合物

生成物 1

HCID 58447638HCID 58447638、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 2-(6-thiomorpholinopyridin-3-yl)acetic acid 219-4 (92 mg, 0.39 mmol), 6-(3-fluorophenyl)pyridin-3-amine 219-1 (73 mg, 0.39 mmol), HATU (162 mg, 0.43 mmol) and DIEA (104 μl, 0.6 mmol) in DMF (1.0 ml) was stirred at room temperature overnight. Then it was redistributed between water (30 ml) and ethyl acetate (40 ml). The organic phase was dried over Na2SO4 and concentrated by rotary evaporation. Silica gel column chromatography (with ethyl acetate/hexanes from 1:10 to 2:1 as eluent) gave N-(6-(3-fluorophenyl)pyridin-3-yl)-2-(6-thiomorpholinopyridin-3-yl)acetamide 219-5 as solid.

後処理

  1. dry with materialThe organic phase was dried over Na2SO4
  2. concentrationconcentrated by rotary evaporation

出典と根拠

ORDレコード
ord-c290fb7995cf4df59aa8440b35a38b62
出典データセット
uspto-grants-2013_10
特許番号
US08546396B2

反応ノート

読み込み中…