Diethyl Ether → HCID 178512745, 화합물

HRID 915792

반응식

HRID 915792 반응식
[NH2:1][CH2:2][C:3]1[CH:16]=[CH:15][C:14]2[O:13][C:12]3[C:7]4=[C:8]([C:17](=[O:20])[NH:18][N:19]=[C:6]4[C:5]=2[CH:4]=1)[CH:9]=[CH:10][CH:11]=3.C(N(C(C)C)CC)(C)C.Cl.N1C=CC([C:36]([NH2:38])=[NH:37])=N1.C(OCC)C>CN(C=O)C>[O:20]=[C:17]1[C:8]2[CH:9]=[CH:10][CH:11]=[C:12]3[O:13][C:14]4[CH:15]=[CH:16][C:3]([CH2:2][NH:1][C:36]([NH2:38])=[NH:37])=[CH:4][C:5]=4[C:6]([C:7]=23)=[N:19][NH:18]1

참가 물질

6

반응물 4

HCID 3283Diethyl EtherHCID 81531DiisopropylethylamineHCID 1119635510-(Aminomethyl)[1]benzopyrano[4,3,2-de]phthalazin-3(2H)-oneHCID 178479321HCID 178479321, 화합물

생성물 1

HCID 178512745HCID 178512745, 화합물수율 94.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To the solution of 49 (0.10 g, 0.38 mmol) in DMF (5 mL) was added diisopropyl ethylamine (0.83 mmol) and 1H-pyrazole carboxamidine hydrochloride (0.12 g, 0.81 mmol). The reaction mixture was stirred at room temperature overnight. Diethyl ether was added to form a white precipitate. The precipitate was collected and recrystallized in EtOAc to afford a white solid 50 (0.11 g, 83%, HCl salt). MS (ES−): 306; 1H-NMR (DMSO-d6, 400 MHz): 12.62 (s, 1H), 8.04 (d, J=2.0 Hz, 1H), 7.92-7.84 (m, 2H), 7.71 (dd, J=7.5 and 2.0 Hz, 1H), 7.50 (dd, J=8.5 and 2.0 Hz, 1H), 7.45 (d, J=8.5 Hz, 1H), 4.47 (s, 2H); Anal. Calcd. for C16H13N5O2.1ClH: C, 55.58; H, 4.27; N, 19.76; Cl, 10.38. Found: C, 55.94; H, 4.17; N, 19.32; Cl, 10.12.

후처리

  1. customto form a white precipitate
  2. customThe precipitate was collected
  3. customrecrystallized in EtOAc

출처 및 근거

ORD 기록
ord-28701d82ae4145e985f185bd40be0e7f
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07268138B2

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