Hydrogen Peroxide → HCID 13646636、化合物

HRID 647107ノート

反応式

HRID 647107 の反応式
[CH3:1][S:2][C:3]1[NH:4][CH:5]=[C:6]([CH2:11][CH2:12][CH2:13][CH3:14])[C:7]=1[N+:8]([O-:10])=[O:9].[OH:15]O>C(O)(=O)C>[CH3:1][S:2]([C:3]1[NH:4][CH:5]=[C:6]([CH2:11][CH2:12][CH2:13][CH3:14])[C:7]=1[N+:8]([O-:10])=[O:9])=[O:15]

参加物

4

反応物 2

HCID 784Hydrogen PeroxideHCID 23325026HCID 23325026、化合物

生成物 1

HCID 13646636HCID 13646636、化合物収率 40.2%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

2-Methylthio-3-nitro-4-n-butylpyrrole (3.7 g) was suspended in glacial acetic acid (50 ml) and 30% hydrogen peroxide (1.62 g) was added. The mixture was heated to 80° for 7 hours, and it was then evaporated to a brown oil. The crude product was purified by column chromatography using silica gel, eluted with benzene and chloroform, to give an oil which crystallized on standing. This was recrystallised from 2-propanol to give 2-methylsulphinyl-3-nitro-4-n-butylpyrrole (1.6 g), m.p. 133°-4°.

後処理

  1. temperatureThe mixture was heated to 80° for 7 hours
  2. customit was then evaporated to a brown oil
  3. customThe crude product was purified by column chromatography
  4. washeluted with benzene and chloroform
  5. customto give an oil which
  6. customcrystallized
  7. customThis was recrystallised from 2-propanol

出典と根拠

ORDレコード
ord-62ff4c7e83a44f36b592d48aecb1272f
出典データセット
uspto-grants-1983_10
特許番号
US04407808

反応ノート

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