Butylamine → HCID 178448799, 화합물

HRID 1604906노트

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HRID 1604906 반응식
Cl[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[N+:3]=1[O-:9].[CH2:10]([NH2:14])[CH2:11][CH2:12][CH3:13]>CS(C)=O>[Cl:8][C:4]1[N+:3]([O-:9])=[C:2]([NH:14][CH2:10][CH2:11][CH2:12][CH3:13])[CH:7]=[CH:6][CH:5]=1

참가 물질

4

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HCID 8007ButylamineHCID 8176732,6-Dichloropyridine N-Oxide

생성물 1

HCID 178448799HCID 178448799, 화합물

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

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온도
120 °C

실험 절차

To a solution consisting of 9.9 grams (0.055 mole) of 2,6-dichloropyridine-N-oxide in 50 milliliters of dimethylsulfoxide was slowly added 8.4 grams (0.115 mole) of n-butylamine. The temperature of the mixture was 75°C. at the start of the reaction and was allowed to increase to 120°C. After a total reaction time of ~21/2 hours, 3/4 of the dimethyl sulfoxide was removed by evaporation and the reaction mixture poured into cold water. The solid 6-chloro-2-(n-butylamino)pyridine-N-oxide product which precipitated was recovered by filtration in the yield of 6.0 grams. The product melted was 103°-104°C. and was found upon analysis to have carbon, hydrogen, chlorine and contents of 54.1, 6.9, 17.9 and 13.8 percent, respectively, as compared with the theoretical contents of 54.0, 6.5, 17.8 and 14.0 percent, respectively, calculated for the above named compound.

후처리

  1. customThe temperature of the mixture was 75°C. at the start of the reaction
  2. customAfter a total reaction time of ~21/2 hours, 3/4 of the dimethyl sulfoxide was removed by evaporation
  3. additionthe reaction mixture poured into cold water
  4. customThe solid 6-chloro-2-(n-butylamino)pyridine-N-oxide product which precipitated
  5. filtrationwas recovered by filtration in the yield of 6.0 grams
  6. custommelted was 103°-104°C.

출처 및 근거

ORD 기록
ord-8d0bcdd96eb241589a3958b821ff9996
출처 데이터셋
uspto-grants-1976_04
특허 번호
US03948910

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