Water → (3,4-Dichlorobenzyl)-(2-methyl-8-morpholin-4-yl-quinolin-4-yl)-amine hydrobromide

HRID 1966512ノート

反応式

HRID 1966512 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:19]=[CH:20][C:21]=1[Cl:22])[CH2:5][NH:6][C:7]1[C:16]2[C:11](=[C:12]([NH2:17])[CH:13]=[CH:14][CH:15]=2)[N:10]=[C:9]([CH3:18])[CH:8]=1.[Br:23][CH2:24][CH2:25][O:26][CH2:27][CH2:28]Br.O>CN(C)C=O>[BrH:23].[Cl:1][C:2]1[CH:3]=[C:4]([CH:19]=[CH:20][C:21]=1[Cl:22])[CH2:5][NH:6][C:7]1[C:16]2[C:11](=[C:12]([N:17]3[CH2:28][CH2:27][O:26][CH2:25][CH2:24]3)[CH:13]=[CH:14][CH:15]=2)[N:10]=[C:9]([CH3:18])[CH:8]=1

参加物

5

反応物 3

HCID 962WaterHCID 21521Bis(2-bromoethyl) etherHCID 59474762N*4*-(3,4-Dichlorobenzyl)-2-methylquinoline-4,8-diamine

生成物 1

HCID 68494369(3,4-Dichlorobenzyl)-(2-methyl-8-morpholin-4-yl-quinolin-4-yl)-amine hydrobromide収率 17.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

N*4*-(3,4-Dichlorobenzyl)-2-methylquinoline-4,8-diamine (60.0 mg, 0.181 mmole) and bis(2-bromoethyl)ether (83.7 mg, 0.361 mmole) in dimethylformamide (1 mL), were stirred at 100° C. for 90 min in a microwave oven. Water was added and the mixture was extracted with dichloromethane. The organic phases were washed with saturated NaCl solution, dried and the solvent was removed. The residue thus obtained was purified using silica gel chromatography, eluting with dichloromethane:water 90:10. Precipitation in ethyl acetate gave a brownish solid (15 mg, 17%).

後処理

  1. extractionthe mixture was extracted with dichloromethane
  2. washThe organic phases were washed with saturated NaCl solution
  3. customdried
  4. customthe solvent was removed
  5. customThe residue thus obtained
  6. customwas purified
  7. washeluting with dichloromethane:water 90:10
  8. customPrecipitation in ethyl acetate

出典と根拠

ORDレコード
ord-76ccdd7f4bb7404387ac0ae8f053c1fe
出典データセット
uspto-grants-2013_04
特許番号
US08420670B2

反応ノート

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