Hydrochloric Acid → HCID 178488956、化合物

HRID 275790

反応式

HRID 275790 の反応式
[NH2:1][C:2]1[C:7]([NH2:8])=[CH:6][CH:5]=[CH:4][C:3]=1[O:9][CH3:10].[C:11](O)(=O)[CH:12]([CH3:14])[OH:13].Cl.[OH-].[NH4+]>>[OH:13][CH:12]([C:14]1[NH:1][C:2]2[C:3]([O:9][CH3:10])=[CH:4][CH:5]=[CH:6][C:7]=2[N:8]=1)[CH3:11]

参加物

5

反応物 4

HCID 313Hydrochloric AcidHCID 612Lactic AcidHCID 14923Ammonium HydroxideHCID 1842683-Methoxybenzene-1,2-diamine

生成物 1

HCID 178488956HCID 178488956、化合物

反応条件

温度
100 °C

実験手順

2,3-Diaminoanisole (5.88 g) and lactic acid (5.6 ml) were combined, treated with concentrated hydrochloric acid (45 ml) and heated at 100° C. for 18 h. The reaction was cooled to 0° C., neutralised with ammonium hydroxide solution and extracted with ethyl acetate (3×45 ml). The combined organic layers were dried over magnesium sulphate, filtered and the filtrate evaporated in vacuo and the residue purified by flash chromatography on silica eluting with ethyl acetate to yield the desired product as a reddish-brown solid (4.91 g).

後処理

  1. temperatureThe reaction was cooled to 0° C.
  2. extractionextracted with ethyl acetate (3×45 ml)
  3. dry with materialThe combined organic layers were dried over magnesium sulphate
  4. filtrationfiltered
  5. customthe filtrate evaporated in vacuo
  6. customthe residue purified by flash chromatography on silica eluting with ethyl acetate

出典と根拠

ORDレコード
ord-5b28579291ae4976832c8cc0540a95c1
出典データセット
uspto-grants-2002_03
特許番号
US06353010B1

関連ノート

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