Hydrazine hydrate (1:1) → HCID 59309723、化合物

HRID 1512988ノート

反応式

HRID 1512988 の反応式
[Cl:1][C:2]1[C:3]([N:11]2C(=O)C3C(=CC=CC=3)C2=O)=[CH:4][C:5]([SH:10])=[C:6]([O:8][CH3:9])[CH:7]=1.O.NN>O1CCCC1>[Cl:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[C:5]([SH:10])=[CH:4][C:3]=1[NH2:11]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 59310058HCID 59310058、化合物

生成物 1

HCID 59309723HCID 59309723、化合物収率 77.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 5-chloro-4-(1,3-dioxo-1,3-dihydroisoindol-2-yl)-2-mercaptoanisole (0.65 g) in tetrahydrofuran (20 mL) was added hydrazine monohydrate (0.5 mL), and the mixture was heated at reflux for 1.5 hours. The insoluble material was removed by filtration, and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (eluent: n-hexane−n-hexane/ethyl acetate=1/1) to give the title compound (0.3 g).

後処理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 1.5 hours
  3. customThe insoluble material was removed by filtration
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe residue was purified by column chromatography on silica gel (eluent: n-hexane−n-hexane/ethyl acetate=1/1)

出典と根拠

ORDレコード
ord-2b7a1a65ef164af5b1452f02e381f2e5
出典データセット
uspto-grants-2012_07
特許番号
US08217069B2

反応ノート

読み込み中…