Sulfuric Acid → HCID 178526297、化合物

HRID 341791ノート

反応式

HRID 341791 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 178526297HCID 178526297、化合物収率 63%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

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.

後処理

  1. customOne leaves
  2. customrecrystallises from glacial acetic acid

出典と根拠

ORDレコード
ord-e00ca9f02f4b4c2d9b2a7c3f4db76525
出典データセット
uspto-grants-1999_01
特許番号
US05856325

反応ノート

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