Hydrochloric Acid → 1,4-Dihydro-6,7-dichloro-5-[5-(N,N-dimethylaminomethyl)-1,2,3-benzotriazol-1-ylmethyl]quinoxalin-2,3-dione

HRID 1957115ノート

反応式

HRID 1957115 の反応式
[Cl:1][C:2]1[C:3]([CH2:17][N:18]2[C:22]3[CH:23]=[CH:24][C:25]([CH2:27][N:28]([CH3:30])[CH3:29])=[CH:26][C:21]=3[N:20]=[N:19]2)=[C:4]2[C:9](=[CH:10][C:11]=1[Cl:12])[N:8]=[C:7]([O:13]C)[C:6]([O:15]C)=[N:5]2.Cl>O1CCOCC1>[Cl:1][C:2]1[C:3]([CH2:17][N:18]2[C:22]3[CH:23]=[CH:24][C:25]([CH2:27][N:28]([CH3:30])[CH3:29])=[CH:26][C:21]=3[N:20]=[N:19]2)=[C:4]2[C:9](=[CH:10][C:11]=1[Cl:12])[NH:8][C:7](=[O:13])[C:6](=[O:15])[NH:5]2

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 543919756,7-dichloro-2,3-dimethoxy-5-[5-(N,N-dimethylaminomethyl)-1,2,3-benzotriazol-1-ylmethyl]quinoxaline

生成物 1

HCID 190688961,4-Dihydro-6,7-dichloro-5-[5-(N,N-dimethylaminomethyl)-1,2,3-benzotriazol-1-ylmethyl]quinoxalin-2,3-dione収率 94%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A mixture of 6,7-dichloro-2,3-dimethoxy-5-[5-(N,N-dimethylaminomethyl)-1,2,3-benzotriazol-1-ylmethyl]quinoxaline (Preparation 24, 110 mg, 0.25 mmol), 2M hydrochloric acid (10 mL) and dioxane (10 mL) was heated at reflux for 5.5 hours. The mixture was concentrated under reduced pressure, diluted with acetone (10 mL) and filtered. The solid was dried under vacuum to give the title compound as an off-white solid (97 mg, 94%), mp 282° C. Found: C, 45.57; H, 4.00; N, 17.67. C18H16Cl2N6 O2. HCl.H2O requires C, 45.64; H, 4.04; N, 17.74%.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 5.5 hours
  3. concentrationThe mixture was concentrated under reduced pressure
  4. additiondiluted with acetone (10 mL)
  5. filtrationfiltered
  6. customThe solid was dried under vacuum

出典と根拠

ORDレコード
ord-b0c66b9f8be8405bb337e333ed816dd8
出典データセット
uspto-grants-1998_07
特許番号
US05783572

反応ノート

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