1,2-Dichloroethane → HCID 10181944、化合物

HRID 460535ノート

反応式

HRID 460535 の反応式
[CH3:1][O:2][C:3](=[O:24])[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:15]=[CH:14][C:13]([NH2:16])=[C:12](C2C=CC(C)=CC=2)[CH:11]=1.[CH:25]1[CH:30]=[CH:29][C:28]([N:31]=[C:32](Cl)Cl)=[CH:27][CH:26]=1.O.Cl[CH2:37][CH2:38]Cl>>[CH3:1][O:2][C:3](=[O:24])[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][O:9][C:10]1[CH:15]=[CH:14][C:13]2[N:16]=[C:32]([NH:31][C:28]3[CH:29]=[CH:30][CH:25]=[CH:26][CH:27]=3)[N:16]([C:13]3[CH:14]=[CH:15][C:37]([CH3:38])=[CH:11][CH:12]=3)[C:12]=2[CH:11]=1

参加物

5

反応物 4

HCID 111,2-DichloroethaneHCID 962WaterHCID 12145Phenylimidocarbonyl chlorideHCID 694348546-[3-(4-Methylphenyl)-4-aminophenyl]oxyhexanoic acid methyl ester

生成物 1

HCID 10181944HCID 10181944、化合物

実験手順

250 mg of 6-[3-(4-methylphenyl)-4-aminophenyl]oxyhexanoic acid methyl ester was dissolved in 1 ml of 1,2-dichloroethane, the solution was mixed with 0.1 ml of phenylisocyanide dichloride, and the mixture was heated for 8 hours to 65° C. After cooling, it was mixed with water, extracted three times with ethyl acetate, the combined organic phases were washed with saturated sodium chloride solution, dried on sodium sulfate and concentrated by evaporation in a vacuum. The residue was crystallized from a mixture that consists of ethyl acetate and diethyl ether. 147 mg was obtained.

後処理

  1. temperaturethe mixture was heated for 8 hours to 65° C
  2. temperatureAfter cooling
  3. extractionextracted three times with ethyl acetate
  4. washthe combined organic phases were washed with saturated sodium chloride solution
  5. customdried on sodium sulfate
  6. concentrationconcentrated by evaporation in a vacuum
  7. customThe residue was crystallized from a mixture that
  8. custom147 mg was obtained

出典と根拠

ORDレコード
ord-fe3a34419aef4d46aa123b2c7cd9d264
出典データセット
uspto-grants-2007_03
特許番号
US07196202B2

反応ノート

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