Triethylamine → HCID 178512293, 화합물

HRID 1383449노트

반응식

HRID 1383449 반응식
[C:1]([NH:3][C:4](=[N:7][C:8]1[CH:13]=[CH:12][N:11]=[CH:10][CH:9]=1)SC)#[N:2].[CH:14]1[C:24]2[CH2:23][CH2:22][C:21]3[CH:25]=[CH:26][CH:27]=[CH:28][C:20]=3[CH:19]([O:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][NH2:35])[C:18]=2[CH:17]=[CH:16][CH:15]=1.C(N(CC)CC)C>N1C=CC=CC=1.C(OCC)C>[CH:25]1[C:21]2[CH2:22][CH2:23][C:24]3[CH:14]=[CH:15][CH:16]=[CH:17][C:18]=3[CH:19]([O:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][NH:35][C:4]([NH:3][C:1]#[N:2])=[N:7][C:8]3[CH:13]=[CH:12][N:11]=[CH:10][CH:9]=3)[C:20]=2[CH:28]=[CH:27][CH:26]=1

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 155219651-Cyano-2-methyl-3-pyridin-4-yl-isothioureaHCID 211877625-(10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-yloxy)-pentylamine

생성물 1

HCID 178512293HCID 178512293, 화합물수율 85%

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 3283Diethyl Ether용매

실험 절차

1-Cyano-2-methyl-3-pyridin-4-yl-isothiourea (573 mg, 3.00 mmol) and 5-(10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-yloxy)-pentylamine (886 mg, 3.00 mmol) were dissolved in pyridine (20 mL). Triethylamine (2 mL, 14 mmol) was added followed by (4-dimethylamino)pyridine (5.0 mg, 0.04 mmol). The reaction mixture was stirred at 86□ C. for 12 hours. After cooling to room temperature, the reaction mixture was diluted with diethyl ether (50 mL). The resulting precipitate was collected by filtration and washed with diethyl ether. The crude product was recrystalized from methanol and diethyl ether to give the desired product as a white crystalline solid (yield 85%). 1H NMR (CDCl3, ppm): 8.54 (dd, 2H), 7.41-7.12 (m, 10H), 5.29 (s, 1H), 3.56-3.41 (m, 4H), 3.32 (dd, 2H), 3.05-2.95 (m, 2H), 1.71-1.41 (m, 6H).

후처리

  1. filtrationThe resulting precipitate was collected by filtration
  2. washwashed with diethyl ether
  3. customThe crude product was recrystalized from methanol and diethyl ether

출처 및 근거

ORD 기록
ord-a00b398a02d0438cb7b8d745f9694f8e
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06255323B1

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