p-Toluenesulfonic acid → HCID 68988102、化合物

HRID 69461ノート

反応式

HRID 69461 の反応式
O1[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][CH2:27][C@@H:28]6[CH2:32][CH2:31][CH2:30][O:29]6)[CH:22]=5)[C:17]4=[O:33])=[CH:12][C:11]=3[F:34])[CH2:6]2)[O:4]CC1.C1(C)C=CC(S(O)(=O)=O)=CC=1>CC(C)=O.O>[F:34][C:11]1[CH:12]=[C:13]([N:16]2[CH2:25][CH2:24][C:23]3[C:18](=[CH:19][CH:20]=[C:21]([O:26][CH2:27][C@@H:28]4[CH2:32][CH2:31][CH2:30][O:29]4)[CH:22]=3)[C:17]2=[O:33])[CH:14]=[CH:15][C:10]=1[N:7]1[CH2:8][CH2:9][C:5](=[O:4])[CH2:6]1

参加物

4

反応物 2

HCID 6101p-Toluenesulfonic acidHCID 68992282HCID 68992282、化合物

生成物 1

HCID 68988102HCID 68988102、化合物

試薬・触媒・溶媒 1

HCID 18366337Propan-2-one--water (1/1)溶媒

反応条件

温度
70 °C

実験手順

A mixture of 2-[4-(1,4-dioxa-7-aza-spiro[4.4]non-7-yl)-3-fluorophenyl]-6-[(S)-1-(tetrahydrofuran-2-yl)methoxy]-3,4-dihydro-2H-isoquinolin-1-one (8.4 g) and p-toluenesulfonic acid (3.4 g) in acetone/water (80 mL/40 mL) was heated for 12 h at 70° C. Then the acetone was removed in vacuum and the aqueous phase was neutralized with sodium hydrogencarbonate solution and then extracted several times with ethyl acetate. The organic phases were combined, dried over sodium sulfate and the solvent was removed in vacuum. In this way the product was obtained with molecular weight 424.47 (C24H25FN2O4); MS (ESI): 425 (M+H+).

後処理

  1. customThen the acetone was removed in vacuum
  2. extractionextracted several times with ethyl acetate
  3. dry with materialdried over sodium sulfate
  4. customthe solvent was removed in vacuum
  5. customIn this way the product was obtained with molecular weight 424.47 (C24H25FN2O4)

出典と根拠

ORDレコード
ord-ad83ca4a916b450ea9ee7c3e86fcb9db
出典データセット
uspto-grants-2014_09
特許番号
US08822495B2

反応ノート

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