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

HRID 48251노트

반응식

HRID 48251 반응식
[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

참가 물질

4

반응물 2

HCID 8022Ethyl isocyanate2회HCID 99443944-(6,8-Dichloro-2-methyl-1,2,3,4-tetrahydroisoquinolin-4-yl)aniline

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매2회

반응 조건

온도
80 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-41ba9da4815a49be819dd54376093c4e
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06703405B2

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