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

HRID 1977539노트

반응식

HRID 1977539 반응식
[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]

참가 물질

7

반응물 3

HCID 10340Sodium CarbonateHCID 21993243n-Sec-butyl-n-ethyl-4-nitroso-3-toluidineHCID 178516258HCID 178516258, 화합물

생성물 1

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

시약·촉매·용매 3

HCID 23925Iron촉매2회HCID 313Hydrochloric Acid용매HCID 887Methanol용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-07c4917aba174374bbdaf7185009b95a
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06235096B1

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