HCID 59612419, 화합물 → [5-(2-Methoxymethyl-phenyl)-[1,2,4]triazolo[1,5-a]pyridin-2-yl]-(2,3,4,5-tetrahydro-1H-benzo[d]azepin-7-yl)-amine

HRID 1890000노트

반응식

HRID 1890000 반응식
C(OC([N:8]1[CH2:14][CH2:13][C:12]2[CH:15]=[C:16]([NH:19][C:20]3[N:37]=[C:23]4[CH:24]=[CH:25][CH:26]=[C:27]([C:28]5[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=5[CH2:34][O:35][CH3:36])[N:22]4[N:21]=3)[CH:17]=[CH:18][C:11]=2[CH2:10][CH2:9]1)=O)(C)(C)C>FC(F)(F)C(O)=O.ClCCl>[CH3:36][O:35][CH2:34][C:29]1[CH:30]=[CH:31][CH:32]=[CH:33][C:28]=1[C:27]1[N:22]2[N:21]=[C:20]([NH:19][C:16]3[CH:17]=[CH:18][C:11]4[CH2:10][CH2:9][NH:8][CH2:14][CH2:13][C:12]=4[CH:15]=3)[N:37]=[C:23]2[CH:24]=[CH:25][CH:26]=1

참가 물질

4

반응물 1

HCID 59612419HCID 59612419, 화합물

생성물 1

HCID 59612550[5-(2-Methoxymethyl-phenyl)-[1,2,4]triazolo[1,5-a]pyridin-2-yl]-(2,3,4,5-tetrahydro-1H-benzo[d]azepin-7-yl)-amine수율 94.2%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 6422Trifluoroacetic acid용매

실험 절차

7-[5-(2-Methoxymethyl-phenyl)-[1,2,4]triazolo[1,5-a]pyridin-2-ylamino]-1,2,4,5-tetrahydro-benzo[d]azepine-3-carboxylic acid tert-butyl ester (105.0 mg, 0.210 mmol) was stirred in 3M trifluoroacetic acid in dichloromethane (10 mL) for 30 minutes. The volatiles were evaporated and the residue was dissolved in ethyl acetate and washed with sodium carbonate solution (2×) and brine. The organic layer was dried over sodium sulfate, filtered and concentrated. Product isolated as a foam (0.079 g, 89%). 1H NMR (400 MHz, CDCl3, δ, ppm): 7.64 (d, J=7.7 Hz, 1H), 7.58-7.41 (m, 5H), 7.25-7.21 (m, 1H), 7.16-7.04 (m, 1H), 6.99 (d, J=8.0 Hz, 1H), 6.91-6.87 (m, 1H), 4.35 (br s, 2H), 3.20 (s, 3H), 2.98-2.81 (m, 8H), 2.02 (br s, 1H). MS=400 (MH)+.

후처리

  1. customThe volatiles were evaporated
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washwashed with sodium carbonate solution (2×) and brine
  4. dry with materialThe organic layer was dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-fd4cb99a9128437096fa020dc1432e55
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08501936B2

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