Diisopropylethylamine → HCID 117727718、化合物

HRID 61268ノート

反応式

HRID 61268 の反応式
[CH3:1][C@@H:2]1[CH2:7][CH2:6][CH2:5][NH:4][C@@H:3]1[CH2:8][N:9]1[C:17](=[O:18])[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10]1=[O:19].[F:20][C:21]1[CH:22]=[C:23]([CH3:31])[C:24]([I:30])=[C:25]([CH:29]=1)[C:26](O)=[O:27].CCN(C(C)C)C(C)C.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>CN(C=O)C.C(OCC)(=O)C>[F:20][C:21]1[CH:22]=[C:23]([CH3:31])[C:24]([I:30])=[C:25]([CH:29]=1)[C:26]([N:4]1[CH2:5][CH2:6][CH2:7][C@@H:2]([CH3:1])[C@H:3]1[CH2:8][N:9]1[C:17](=[O:18])[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10]1=[O:19])=[O:27]

参加物

7

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 715354825-Fluoro-2-iodo-3-methylbenzoic acidHCID 1177276302-(((2S,3R)-3-Methylpiperidin-2-yl)methyl)isoindoline-1,3-dione

生成物 1

HCID 117727718HCID 117727718、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 2-(((2S,3R)-3-methylpiperidin-2-yl)methyl)isoindoline-1,3-dione (1.2 eq.), 5-fluoro-2-iodo-3-methylbenzoic acid (1 eq.), DIPEA (3 eq.), and HATU (1 eq.) in DMF (0.2 M) was stirred at rt for 1 h. The reaction mixture was diluted with ethyl acetate and washed with satd. NaHCO3 and brine. The organic layer was separated, dried with MgSO4, and concentrated in vacuo. The crude product was purified by chromatography on silica gel (EtOAc/hexanes) to afford the title compound.

後処理

  1. washwashed with satd
  2. customThe organic layer was separated
  3. dry with materialdried with MgSO4
  4. concentrationconcentrated in vacuo
  5. customThe crude product was purified by chromatography on silica gel (EtOAc/hexanes)

出典と根拠

ORDレコード
ord-59cecee5a26f423eadbd341cd8db4c9b
出典データセット
uspto-grants-2016_09
特許番号
US09440982B2

反応ノート

読み込み中…