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

HRID 126768

반응식

HRID 126768 반응식
[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

참가 물질

5

반응물 3

HCID 7628Boric AcidHCID 167232,4,5,6(1H,3H)-Pyrimidinetetrone, monohydrateHCID 792974,5-Dichloro-1,2-phenylenediamine

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-fb47faf0040341b8bd2c4fd54bb0c4b5
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04254123

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