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

HRID 1957115노트

반응식

HRID 1957115 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-b0c66b9f8be8405bb337e333ed816dd8
출처 데이터셋
uspto-grants-1998_07
특허 번호
US05783572

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