Hydrochloric Acid → 8-iodo-2,3,4,5-tetrahydro-1H-1-benzazepine-2,5-dione

HRID 2387972ノート

反応式

HRID 2387972 の反応式
[I:1][C:2]1[CH:18]=[CH:17][C:5]2[C:6](=[O:16])[CH:7](C(OC)=O)[CH2:8][C:9](=[O:11])[NH:10][C:4]=2[CH:3]=1.Cl>CS(C)=O.O>[I:1][C:2]1[CH:18]=[CH:17][C:5]2[C:6](=[O:16])[CH2:7][CH2:8][C:9](=[O:11])[NH:10][C:4]=2[CH:3]=1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 58476574methyl 8-iodo-2,5-dioxo-2,3,4,5-tetrahydro-1H-1-benzazepine-4-carboxylate

生成物 1

HCID 584766238-iodo-2,3,4,5-tetrahydro-1H-1-benzazepine-2,5-dione収率 99.6%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 962Water溶媒

反応条件

温度
150 °C

実験手順

A mixture of methyl 8-iodo-2,5-dioxo-2,3,4,5-tetrahydro-1H-1-benzazepine-4-carboxylate (74 g, 0.2 mol) in DMSO (560 mL) and H2O (16 mL) was heated at 150° C. for 4 h. The reaction mixture was allowed to cool to rt, ice (1.0 L) was added, and the mixture was allowed to stir 12 h. To the flask was added 1N HCl (1.0 L) at 0° C. and the mixture allowed to stir for 3 h. The resulting precipitate was filtered and dried under reduced pressure to afford 8-iodo-3,4-dihydro-1H-1-benzazepine-2,5-dione (60 g, 97%).

後処理

  1. temperatureto cool to rt
  2. stirringto stir for 3 h
  3. filtrationThe resulting precipitate was filtered
  4. customdried under reduced pressure

出典と根拠

ORDレコード
ord-d1c91e1f8944416685dbd768794dd58d
出典データセット
uspto-grants-2012_09
特許番号
US08268992B2

反応ノート

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