p-Toluenesulfonic acid → HCID 68988088、化合物

HRID 69419ノート

反応式

HRID 69419 の反応式
[CH2:1]([O:5][C:6]1[CH:7]=[C:8]2[C:13](=[CH:14][CH:15]=1)[C:12](=[O:16])[N:11]([C:17]1[CH:22]=[CH:21][C:20]([N:23]3[CH2:31][CH2:30][C:25]4(OCC[O:26]4)[CH2:24]3)=[CH:19][CH:18]=1)[CH2:10][CH2:9]2)[CH2:2][CH2:3][CH3:4].C1(C)C=CC(S(O)(=O)=O)=CC=1>CC(C)=O>[CH2:1]([O:5][C:6]1[CH:7]=[C:8]2[C:13](=[CH:14][CH:15]=1)[C:12](=[O:16])[N:11]([C:17]1[CH:22]=[CH:21][C:20]([N:23]3[CH2:31][CH2:30][C:25](=[O:26])[CH2:24]3)=[CH:19][CH:18]=1)[CH2:10][CH2:9]2)[CH2:2][CH2:3][CH3:4]

参加物

4

反応物 2

HCID 6101p-Toluenesulfonic acidHCID 689920606-butoxy-2-[4-(1,4-dioxa-7-azaspiro[4.4]non-7-yl)phenyl]-3,4-dihydro-2H-isoquinolin-1-one

生成物 1

HCID 68988088HCID 68988088、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 6-butoxy-2-[4-(1,4-dioxa-7-azaspiro[4.4]non-7-yl)phenyl]-3,4-dihydro-2H-isoquinolin-1-one (1.40 g), p-toluenesulfonic acid (57 mg) and acetone (40 mL) was boiled under reflux for 12 hours and then concentrated. The residue was partitioned between sodium carbonate solution and ethyl acetate. The organic phase was dried and concentrated. The product with the molecular weight of 378.48 (C23H26N2O3) was obtained in this way; MS (ESI): 379 (M+H+).

後処理

  1. temperatureunder reflux for 12 hours
  2. concentrationconcentrated
  3. customThe residue was partitioned between sodium carbonate solution and ethyl acetate
  4. customThe organic phase was dried
  5. concentrationconcentrated
  6. customThe product with the molecular weight of 378.48 (C23H26N2O3) was obtained in this way

出典と根拠

ORDレコード
ord-6dfa129263f14983beed32c30c97c363
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…