4-Bromobenzyl isocyanate → HCID 11740716, 화합물

HRID 585999

반응식

HRID 585999 반응식
[CH3:1][C:2]1[C:11]2[CH:10]=[CH:9][CH:8]=[C:7]([NH2:12])[C:6]=2[CH:5]=[C:4]([CH3:13])[N:3]=1.[Br:14][C:15]1[CH:20]=[CH:19][C:18]([CH2:21][N:22]=[C:23]=[O:24])=[CH:17][CH:16]=1>C1(C)C=CC=CC=1>[Br:14][C:15]1[CH:16]=[CH:17][C:18]([CH2:21][NH:22][C:23]([NH:12][C:7]2[CH:8]=[CH:9][CH:10]=[C:11]3[C:6]=2[CH:5]=[C:4]([CH3:13])[N:3]=[C:2]3[CH3:1])=[O:24])=[CH:19][CH:20]=1

참가 물질

4

반응물 2

HCID 43746174-Bromobenzyl isocyanateHCID 223376241,3-Dimethylisoquinolin-5-amine

생성물 1

HCID 11740716HCID 11740716, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
87.5 °C

실험 절차

The product from Example 178A (375 mg, 2.2 mmol) in toluene (7 mL) was treated with 1-bromo-4-(isocyanatomethyl)benzene (0.31 mL, 2.2 mmol). After stirring at 85-90° C. for 3 hours, the mixture was cooled to room temperature and filtered. The filter cake was treated with methanolic HCl to provide the title compound as the hydrochloride salt. 1H NMR (300 MHz, DMSO-d6) δ 8.62 (s, 1H), 8.17 (d, 1H, J=7.8 Hz), 7.80 (d, 1H, J=8.5 Hz), 7.45-7.60 (m, 4H), 7.32 (d, 2H, J=8.1 Hz), 7.06 (t, 1H, 5.7 Hz), 4.34 (d, 2H, 5.8 Hz), 2.84 (s, 3H), 2.75 (s, 3H); MS (ESI+) m/z 383/385 (M+H, 79Br/81Br).

후처리

  1. temperaturethe mixture was cooled to room temperature
  2. filtrationfiltered
  3. additionThe filter cake was treated with methanolic HCl

출처 및 근거

ORD 기록
ord-db9150ea86aa433e8c1de95b85530479
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06933311B2

연결된 노트

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