Triethylamine → 2-Bromo-N-(6-methyl-pyridazin-3-yl)-acetamide

HRID 2192376노트

반응식

HRID 2192376 반응식
[Br:1][CH2:2][C:3](Br)=[O:4].[NH2:6][C:7]1[N:8]=[N:9][C:10]([CH3:13])=[CH:11][CH:12]=1.C(N(CC)CC)C>C(Cl)(Cl)Cl>[Br:1][CH2:2][C:3]([NH:6][C:7]1[N:8]=[N:9][C:10]([CH3:13])=[CH:11][CH:12]=1)=[O:4]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 61147Bromoacetyl bromideHCID 877126-Methylpyridazin-3-amine

생성물 1

HCID 673108012-Bromo-N-(6-methyl-pyridazin-3-yl)-acetamide

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

A solution of bromoacetyl bromide (0.22 mL) in dry CHCl3 (4 mL) was added slowly to a suspension of 3-amino-6-methylpyridazine (0.24 g) and triethylamine (0.47 mL) in dry CHCl3 (45 mL) at room temperature. The brown mixture was allowed to stir for 3.5 hr, then quenched with H2O (1.5 mL) and stirred for 20 mins before concentrating under reduced pressure to a brown solid. The crude product was purified by silica gel chromatography eluting with 1-2% MeOH/dichloromethane. The relevant fractions were combined and evaporated to give the title compound (0.20 g) as a pinkish/beige solid.

후처리

  1. customquenched with H2O (1.5 mL)
  2. stirringstirred for 20 mins
  3. concentrationbefore concentrating under reduced pressure to a brown solid
  4. customThe crude product was purified by silica gel chromatography
  5. washeluting with 1-2% MeOH/dichloromethane
  6. customevaporated

출처 및 근거

ORD 기록
ord-f936bb35d18b4f92b12d235e0b7d0eff
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08329729B2

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