4-Bromo-2-methoxy-6-methylaniline → N-(4-Bromo-2-methoxy-6-methylphenyl)-7-(2-ethyl-1-piperidinyl)-1-methyl-1H-benzimidazol-2-amine

HRID 2235562노트

반응식

HRID 2235562 반응식
Cl[C:2]1[N:6]([CH3:7])[C:5]2[C:8]([N:12]3[CH2:17][CH2:16][CH2:15][CH2:14][CH:13]3[CH2:18][CH3:19])=[CH:9][CH:10]=[CH:11][C:4]=2[N:3]=1.[Br:20][C:21]1[CH:27]=[C:26]([CH3:28])[C:24]([NH2:25])=[C:23]([O:29][CH3:30])[CH:22]=1>C(OCC)(=O)C>[Br:20][C:21]1[CH:27]=[C:26]([CH3:28])[C:24]([NH:25][C:2]2[N:6]([CH3:7])[C:5]3[C:8]([N:12]4[CH2:17][CH2:16][CH2:15][CH2:14][CH:13]4[CH2:18][CH3:19])=[CH:9][CH:10]=[CH:11][C:4]=3[N:3]=2)=[C:23]([O:29][CH3:30])[CH:22]=1

참가 물질

4

반응물 2

HCID 106802184-Bromo-2-methoxy-6-methylanilineHCID 685813412-Chloro-7-(2-ethyl-1-piperidinyl)-1-methyl-1H-benzimidazole

생성물 1

HCID 58896452N-(4-Bromo-2-methoxy-6-methylphenyl)-7-(2-ethyl-1-piperidinyl)-1-methyl-1H-benzimidazol-2-amine수율 30%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
110 °C

실험 절차

A mixture of 2-chloro-7-(2-ethyl-1-piperidinyl)-1-methyl-1H-benzimidazole (100 mg, 0.36 mmol) and 4-bromo-2-methoxy-6-methylaniline (390 mg, 1.8 mmol) was heated at 110° C. for 12 h. The mixture was dissolved in ethyl acetate and washed with saturated sodium bicarbonate in water, dried over magnesium sulfate and concentrated under vacuum. The residue was purified by column chromatography eluting with a 15% acetone/hexanes mixture to afford 49.3 mg (30%) of the title compound.

후처리

  1. washwashed with saturated sodium bicarbonate in water
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated under vacuum
  4. customThe residue was purified by column chromatography
  5. washeluting with a 15% acetone/hexanes mixture

출처 및 근거

ORD 기록
ord-83f0d8b955794d2b902f749bd4fd511e
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07714009B2

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