2,4-Difluorophenyl isocyanate → N-[4-(2-chlorophenyl)-2-ethylthieno[2,3-b]pyridin-5-yl]-N'-(2,4-difluorophenyl)urea

HRID 1657219노트

반응식

HRID 1657219 반응식
[NH2:1][C:2]1[C:3]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[Cl:19])=[C:4]2[CH:10]=[C:9]([CH2:11][CH3:12])[S:8][C:5]2=[N:6][CH:7]=1.[F:20][C:21]1[CH:26]=[C:25]([F:27])[CH:24]=[CH:23][C:22]=1[N:28]=[C:29]=[O:30]>O1CCCC1>[Cl:19][C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=1[C:3]1[C:2]([NH:1][C:29]([NH:28][C:22]2[CH:23]=[CH:24][C:25]([F:27])=[CH:26][C:21]=2[F:20])=[O:30])=[CH:7][N:6]=[C:5]2[S:8][C:9]([CH2:11][CH3:12])=[CH:10][C:4]=12

참가 물질

4

반응물 2

HCID 5932582,4-Difluorophenyl isocyanateHCID 197871805-Amino-4-(2-chlorophenyl)-2-ethylthieno[2,3-b]pyridine

생성물 1

HCID 9889640N-[4-(2-chlorophenyl)-2-ethylthieno[2,3-b]pyridin-5-yl]-N'-(2,4-difluorophenyl)urea수율 93.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 5-amino-4-(2-chlorophenyl)-2-ethylthieno[2,3-b]pyridine (288 mg) in tetrahydrofuran (3 ml) was added 2,4-difluorophenyl isocyanate (0.13 ml) and the mixture was stirred at room temperature for 18 hours, and then the solvent was distilled off. To the residue was added isopropyl ether to obtain N-[4-(2-chlorophenyl)-2-ethylthieno[2,3-b]pyridin-5-yl]-N'-(2,4-difluorophenyl)urea as crystals (416 mg, 93.9 %). Colorless prisms were obtained by recrystallization from acetone-hexane, mp: 217°-218° C.

후처리

  1. distillationthe solvent was distilled off
  2. additionTo the residue was added isopropyl ether

출처 및 근거

ORD 기록
ord-b192eb97969f4c4e9ef803e89ab51ffc
출처 데이터셋
uspto-grants-1993_10
특허 번호
US05256782

반응 노트

불러오는 중…