Sulfuric Acid → HCID 178526297, 화합물

HRID 341791노트

반응식

HRID 341791 반응식
[N+:1]1([O-:12])[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[N:4]=[C:3](N)[N:2]=1.S(=O)(=O)(O)[OH:14].N([O-])=O.[Na+].CCOCC>O>[N+:1]1([O-:12])[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[N:4]=[C:3]([OH:14])[N:2]=1

참가 물질

6

반응물 4

HCID 1118Sulfuric AcidHCID 3283Diethyl EtherHCID 794701,2,4-Benzotriazin-3-amine, 1-oxideHCID 23668193Sodium Nitrite

생성물 1

HCID 178526297HCID 178526297, 화합물수율 63%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

To a solution of 7.5 g (46 mmol) 1,2,4-benzotriazine-3-amine 1-oxide (Chem. Ber. 46, 3522 (1913) in 75 ml water and 27 ml conc. sulphuric acid one adds dropwise at room temp. a solution of 13.3 g sodium nitrite in 25 ml water. One leaves to stand overnight, filters, takes up in soda solution, washes with ether, acidifies the aqueous phase, filters and recrystallises from glacial acetic acid. One isolates 4.7 g of title compound (63% of theory) of the m.p. 238-239° C.

후처리

  1. customOne leaves
  2. customrecrystallises from glacial acetic acid

출처 및 근거

ORD 기록
ord-e00ca9f02f4b4c2d9b2a7c3f4db76525
출처 데이터셋
uspto-grants-1999_01
특허 번호
US05856325

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