反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:7]=[CH:8][CH:9]=1)[NH2:6].[N:10]([O-])=O.[Na+].[Sn].[ClH:15]>O>[ClH:15].[CH3:1][O:2][C:3]1[CH:4]=[C:5]([NH:6][NH2:10])[CH:7]=[CH:8][CH:9]=1参加物
6
実験手順
A suspension of 3-methoxyaniline (10 g) in concentrated hydrochloric acid (85 ml) was stirred at ca. 0° and a solution of sodium nitrite (5.75 g) in water (25 ml) was slowly added over a period of 30 min keeping the temperature of the mixture at ca. 0°. After 1 h a solution of tin II chloride dihydrate (59 g) in concentrated hydrochloric acid (50 ml) was added over a period of 1.5 h, to the cooled suspension keeping the temperature below 0° C. The suspension was stirred for a further 30 min, filtered and washed with dried ether to give the title compound as a solid (14 g) m.p. 171°.
後処理
- customat ca. 0°
- customthe temperature below 0° C
- stirringThe suspension was stirred for a further 30 min
- filtrationfiltered
- washwashed with dried ether
出典と根拠
- ORDレコード
- ord-f29eda88a35249c99e36ce3a1f68295a
- 出典データセット
- uspto-grants-1988_02
- 特許番号
- US04725615
関連ノート
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