Cesium carbonate → HCID 68992282、化合物

HRID 69462ノート

反応式

HRID 69462 の反応式
[O:1]1[C:5]2([CH2:9][CH2:8][N:7]([C:10]3[CH:15]=[CH:14][C:13]([N:16]4[CH2:25][CH2:24][C:23]5[C:18](=[CH:19][CH:20]=[C:21]([OH:26])[CH:22]=5)[C:17]4=[O:27])=[CH:12][C:11]=3[F:28])[CH2:6]2)[O:4][CH2:3][CH2:2]1.CS([CH2:33][C@@H:34]1[CH2:38][CH2:37][CH2:36][O:35]1)(=O)=O.C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C=O)C.C(OCC)(=O)C.O>[O:4]1[C:5]2([CH2:9][CH2:8][N:7]([C:10]3[CH:15]=[CH:14][C:13]([N:16]4[CH2:25][CH2:24][C:23]5[C:18](=[CH:19][CH:20]=[C:21]([O:26][CH2:33][C@@H:34]6[CH2:38][CH2:37][CH2:36][O:35]6)[CH:22]=5)[C:17]4=[O:27])=[CH:12][C:11]=3[F:28])[CH2:6]2)[O:1][CH2:2][CH2:3]1

参加物

7

反応物 3

HCID 10796Cesium carbonateHCID 689879432-[4-(1,4-dioxa-7-aza-spiro[4.4]non-7-yl)-3-fluorophenyl]-6-hydroxy-3,4-dihydro-2H-isoquinolin-1-oneHCID 68988132(S)-2-methanesulfonylmethyl-tetrahydrofuran

生成物 1

HCID 68992282HCID 68992282、化合物

試薬・触媒・溶媒 3

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

反応条件

温度
75 °C

実験手順

A mixture of 2-[4-(1,4-dioxa-7-aza-spiro[4.4]non-7-yl)-3-fluorophenyl]-6-hydroxy-3,4-dihydro-2H-isoquinolin-1-one (6.9 g), (S)-2-methanesulfonylmethyl-tetrahydrofuran (3.9 g) and cesium carbonate (17.6 g) in DMF (81.6 mL) was heated overnight at 75° C. Then the reaction mixture was diluted with ethyl acetate and water. The organic phase was washed several times with water, dried over sodium sulfate and the solvent was removed in vacuum. In this way the product was obtained with molecular weight 468.53 (C26H29FN2O5); MS (ESI): 469 (M+H+).

後処理

  1. washThe organic phase was washed several times with water
  2. dry with materialdried over sodium sulfate
  3. customthe solvent was removed in vacuum
  4. customIn this way the product was obtained with molecular weight 468.53 (C26H29FN2O5)

出典と根拠

ORDレコード
ord-44f8eafca076464e8a27cb328f1a524d
出典データセット
uspto-grants-2014_09
特許番号
US08822495B2

反応ノート

読み込み中…