Ethyl isocyanate → 1-[4-(6,8-Dichloro-2-methyl-1,2,3,4-tetrahydroisoquinolin-4-yl)phenyl]-3-ethylurea, Hydrochloride

HRID 48251ノート

反応式

HRID 48251 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[C:10]([Cl:12])[CH:11]=1)[CH2:8][N:7]([CH3:13])[CH2:6][CH:5]2[C:14]1[CH:19]=[CH:18][C:17]([NH2:20])=[CH:16][CH:15]=1.[CH2:21]([N:23]=[C:24]=[O:25])[CH3:22]>C1(C)C=CC=CC=1>[ClH:1].[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[C:10]([Cl:12])[CH:11]=1)[CH2:8][N:7]([CH3:13])[CH2:6][CH:5]2[C:14]1[CH:19]=[CH:18][C:17]([NH:20][C:24]([NH:23][CH2:21][CH3:22])=[O:25])=[CH:16][CH:15]=1

参加物

4

反応物 2

HCID 8022Ethyl isocyanate2 回HCID 99443944-(6,8-Dichloro-2-methyl-1,2,3,4-tetrahydroisoquinolin-4-yl)aniline

生成物 1

HCID 227430501-[4-(6,8-Dichloro-2-methyl-1,2,3,4-tetrahydroisoquinolin-4-yl)phenyl]-3-ethylurea, Hydrochloride

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

反応条件

温度
80 °C

実験手順

500 mg (1.63 mmol) of 4-(6,8-dichloro-2-methyl-1,2,3,4-tetrahydroisoquinolin-4-yl)phenylamine were introduced into 20 ml of toluene, and a solution of 284 mg (4.0 mmol) of ethyl isocyanate in a little toluene is added dropwise. After one hour at 80° C., a further 180 mg of ethyl isocyanate are added, and the mixture was stirred at 80° C. for one hour. For workup, the solvent was removed and the residue was triturated with H2O and ethyl acetate, filtered off with suction and dried, resulting in the title compound as a pale yellowish solid (m.p.: 218-220° C.). The ethylurea obtained in this way was converted into the corresponding hydrochloride in a manner known to the skilled worker.

後処理

  1. customFor workup, the solvent was removed
  2. customthe residue was triturated with H2O and ethyl acetate
  3. filtrationfiltered off with suction
  4. customdried

出典と根拠

ORDレコード
ord-41ba9da4815a49be819dd54376093c4e
出典データセット
uspto-grants-2004_03
特許番号
US06703405B2

反応ノート

読み込み中…