Trifluoroacetic acid → isoquinoline-1-carboxylic acid {1-[(2-hydroxy-5-oxo-tetra-hydrofuran-3-ylcarbamoyl)methyl]-2-oxo-2,3,4,7-tetrahydro-1H-azepin-3-yl} amide

HRID 891192ノート

反応式

HRID 891192 の反応式
C([O:3][CH:4]1[CH:8]([NH:9][C:10]([CH2:12][N:13]2[CH2:19][CH:18]=[CH:17][CH2:16][CH:15]([NH:20][C:21]([C:23]3[C:32]4[C:27](=[CH:28][CH:29]=[CH:30][CH:31]=4)[CH:26]=[CH:25][N:24]=3)=[O:22])[C:14]2=[O:33])=[O:11])[CH2:7][C:6](=[O:34])[O:5]1)C.FC(F)(F)C(O)=O>CC#N.O>[OH:3][CH:4]1[CH:8]([NH:9][C:10]([CH2:12][N:13]2[CH2:19][CH:18]=[CH:17][CH2:16][CH:15]([NH:20][C:21]([C:23]3[C:32]4[C:27](=[CH:28][CH:29]=[CH:30][CH:31]=4)[CH:26]=[CH:25][N:24]=3)=[O:22])[C:14]2=[O:33])=[O:11])[CH2:7][C:6](=[O:34])[O:5]1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 86590750isoquinoline-1-carboxylic acid {1-[(2-ethoxy-5-oxo-tetra-hydrofuran-3-ylcarbamoyl)methyl]-2-oxo-2,3,4,7-tetrahydro-1H-azepin-3-yl} amide

生成物 1

HCID 75025996isoquinoline-1-carboxylic acid {1-[(2-hydroxy-5-oxo-tetra-hydrofuran-3-ylcarbamoyl)methyl]-2-oxo-2,3,4,7-tetrahydro-1H-azepin-3-yl} amide

試薬・触媒・溶媒 1

HCID 18373917Acetonitrile--water (1/1)溶媒

実験手順

To a solution of isoquinoline-1-carboxylic acid {1-[(2-ethoxy-5-oxo-tetra-hydrofuran-3-ylcarbamoyl)methyl]-2-oxo-2,3,4,7-tetrahydro-1H-azepin-3-yl} amide, 6, from above in CH3CN/H2O is added trifluoroacetic acid. After stirring for 30 minutes the solution is concentrated in vacuo and the crude product purified by preparative reverse phase HPLC to afford the desired product.

後処理

  1. concentrationis concentrated in vacuo
  2. customthe crude product purified by preparative reverse phase HPLC

出典と根拠

ORDレコード
ord-460d2057d4e04209a19a070ff7e863c1
出典データセット
uspto-grants-2006_02
特許番号
US07001899B2

反応ノート

読み込み中…