Ethyl Acetate → HCID 178509156, 화합물

HRID 255002노트

반응식

HRID 255002 반응식
[NH2:1][C:2]1[C:3](=[N:17][NH:18][C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([F:25])[CH:20]=2)[C:4]([CH2:7][NH:8][C:9](=[O:16])[C:10]2C=CC=NC=2)=[N:5][N:6]=1.NCC1C(=NNC2C=CC=C(F)C=2)C(N)=NN=1.Cl.C(Cl)(=O)C1C=CC=NC=1.[C:53]([O:56]CC)(=[O:55])[CH3:54]>>[NH2:1][C:2]1[C:3](=[N:17][NH:18][C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([F:25])[CH:20]=2)[C:4]([CH2:7][NH:8][C:9]([CH:10]=[CH:54][C:53]([OH:56])=[O:55])=[O:16])=[N:5][N:6]=1

참가 물질

5

반응물 4

HCID 8857Ethyl AcetateHCID 884383-Pyridinecarbonyl chloride, hydrochloride (1:1)HCID 178509154HCID 178509154, 화합물HCID 178510679HCID 178510679, 화합물

생성물 1

HCID 178509156HCID 178509156, 화합물수율 41%

실험 절차

In a similar manner, N-{5-amino-4-[(3-fluorophenyl)hydrazono]4H-pyrazol-3-ylmethyl}nicotinamide was prepared by reacting 5-aminomethyl-4-[(3-fluorophenyl)hydrazono]-4H-pyrazol-3-ylamine (60 mg, 0.25 mmole) with nicotinoyl chloride hydrochloride (46.3 mg, 0.26 mmole). The reaction was worked up by the addition of saline and ethyl acetate. The crude material was purified by preparative TLC (CH2Cl2:MeOH=9:1) to yield 36 mg (41%) of the title compound as a yellow powder. MS (m/z, ES+): 340 (M+1, 100%); 1H NMR (ppm, 300 MHz, DMSO-d6) δ 11.80 (br s, 1H), 9.01 (br s, 2H), 8.70 (d, 1H), 8.20 (d, 1H), 7.30-7.70 (m, 4H), 6.85-7.25 (m, 3H), 4.70 (br s, 2H).

후처리

  1. customThe crude material was purified by preparative TLC (CH2Cl2:MeOH=9:1)

출처 및 근거

ORD 기록
ord-912d0977a85c41e5bc8e27a7395a7e54
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07875728B2

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