Sodium Carbonate → 4-Amino-n-sec-butyl-n-ethyl-3-toluidine

HRID 1977539ノート

反応式

HRID 1977539 の反応式
[CH:1]([N:5]([CH2:15][CH3:16])[C:6]1[CH:11]=[CH:10][C:9]([N:12]=O)=[C:8]([CH3:14])[CH:7]=1)([CH2:3][CH3:4])[CH3:2].C(=O)([O-])[O-].[Na+].[Na+].C1C(=NNC2C=CC(/C=C/C3C=CC(NN=C4C=CC(=O)C=C4)=CC=3S([O-])(=O)=O)=C(S([O-])(=O)=O)C=2)C=CC(=O)C=1.[Na+].[Na+]>CO.Cl.[Fe]>[NH2:12][C:9]1[CH:10]=[CH:11][C:6]([N:5]([CH:1]([CH2:3][CH3:4])[CH3:2])[CH2:15][CH3:16])=[CH:7][C:8]=1[CH3:14]

参加物

7

反応物 3

HCID 10340Sodium CarbonateHCID 21993243n-Sec-butyl-n-ethyl-4-nitroso-3-toluidineHCID 178516258HCID 178516258、化合物

生成物 1

HCID 219932414-Amino-n-sec-butyl-n-ethyl-3-toluidine

試薬・触媒・溶媒 3

HCID 23925Iron触媒2 回HCID 313Hydrochloric Acid溶媒HCID 887Methanol溶媒2 回

実験手順

A suspension of iron powder (8.34 g) in methanol (60 ml) and hydrochloric acid (20 ml) was stirred at reflux for 15 mins. A solution of the product from Stage 1d (11 g) in methanol (60 ml) was added dropwise over 15 mins and refluxing continued for 3 hours. Sodium carbonate was added until no soluble iron remained and the solution was alkaline to Brilliant Yellow paper. The hot reaction mixture was filtered and the solvent removed under reduced pressure to give the product as a brown oil.

後処理

  1. temperatureat reflux for 15 mins
  2. temperaturerefluxing
  3. filtrationThe hot reaction mixture was filtered
  4. customthe solvent removed under reduced pressure

出典と根拠

ORDレコード
ord-07c4917aba174374bbdaf7185009b95a
出典データセット
uspto-grants-2001_05
特許番号
US06235096B1

反応ノート

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