硼酸 → Benzo(g)pteridine-2,4(1H,3H)-dione, 7,8-dichloro-

HRID 126768

反应方程式

HRID 126768 反应方程式
[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][C:5]([NH2:9])=[C:4]([NH2:10])[CH:3]=1.O.[NH:12]1[C:20](=[O:21])[C:18](=O)[C:16](=O)[NH:15][C:13]1=[O:14].B(O)(O)O>C(O)(=O)C>[CH:3]1[C:2]([Cl:1])=[C:7]([Cl:8])[CH:6]=[C:5]2[N:9]=[C:16]3[NH:15][C:13](=[O:14])[NH:12][C:20](=[O:21])[C:18]3=[N:10][C:4]=12

参与物

5

反应物 3

HCID 7628硼酸HCID 16723阿脲一水合物HCID 792974,5-二氯-1,2-苯二胺

产物 1

HCID 5487670Benzo(g)pteridine-2,4(1H,3H)-dione, 7,8-dichloro-收率 99.9%

试剂、催化剂与溶剂 1

HCID 176醋酸溶剂

实验过程

A solution of 10 g of 4,5-dichloro-o-phenylenediamine, 9 g of alloxan hydrate, 1.5 g of boric acid and 250 ml of glacial acetic acid was stirred overnight at room temperature to obtain a brown-black solution which was filtered. The yellow-buff crystalline solid was well washed with water to obtain 15.9 g of 7,8-dichloro-alloxazine melting at >370° C. A solution of 2 g of 7,8-dichloro-alloxazine in 10 ml of concentrated sulfuric acid was slowly heated to 240° C. and held there for 10 minutes. The mixture was cooled and poured onto ice and the mixture was made alkaline with sodium hydroxide addition. The mixture was extracted several times with ether to obtain 0.73 g of 2-amino-6,7-dichloro-quinoxaline as an orange crystalline solid melting at 220° C.

后处理

  1. customto obtain a brown-black solution which
  2. filtrationwas filtered
  3. washThe yellow-buff crystalline solid was well washed with water

来源与证据

ORD记录
ord-fb47faf0040341b8bd2c4fd54bb0c4b5
来源数据集
uspto-grants-1981_03
专利号
US04254123

关联笔记

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