Water → HCID 70081578, 화합물

HRID 461339노트

반응식

HRID 461339 반응식
[CH2:1]([N:3]([CH2:6]C)CC)[CH3:2].[CH2:8]([C:15]1[C:20]([NH2:21])=CC=CN=1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.Cl[CH2:23][C:24]([Cl:26])=O.[OH2:27]>C1C=CC=CC=1>[CH2:8]([CH2:15][C:20]([NH:21][C:6]1[C:24]([Cl:26])=[CH:23][CH:2]=[CH:1][N:3]=1)=[O:27])[C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 6577Chloroacetyl chlorideHCID 8471TriethylamineHCID 189526852-Benzylpyridin-3-amine

생성물 1

HCID 70081578HCID 70081578, 화합물수율 92%

시약·촉매·용매 1

HCID 241Benzene용매3회

실험 절차

3.4 ml tri-ethylamine is added to a solution of 4.5 g (0.025 mol) 2-benzyl-3-aminopyridine in 25 ml dry benzene. A solution of 2 ml chloro-acetyl chloride in 40 ml dry benzene is then added with stirring to this solution at a temperature of 5°-10° C. The mixture is stirred for 30 minutes at room temperature and a precipitate forms. This precipitate is redissolved by addition of 50 ml water and 50 ml benzene to the mixture. The organic phase is subsequently separated off, dried, and evaporated to dryness. The residue, a white solid, is recrystallized from a little benzene, giving 5.78 g (92%) 2-benzyl-3-chloro-acetamidopyridine of melting point 145°-147° C.

후처리

  1. stirringThe mixture is stirred for 30 minutes at room temperature
  2. customThe organic phase is subsequently separated off
  3. customdried
  4. customevaporated to dryness
  5. customThe residue, a white solid, is recrystallized from a little benzene

출처 및 근거

ORD 기록
ord-a1c92ce32d7b47cfb539f427963d5278
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04062848

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