Ethyl Acetate → HCID 178509156、化合物

HRID 255002ノート

反応式

HRID 255002 の反応式
[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

参加物

5

反応物 4

HCID 8857Ethyl AcetateHCID 884383-Pyridinecarbonyl chloride, hydrochloride (1:1)HCID 178509154HCID 178509154、化合物HCID 178510679HCID 178510679、化合物

生成物 1

HCID 178509156HCID 178509156、化合物収率 41%

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-912d0977a85c41e5bc8e27a7395a7e54
出典データセット
uspto-grants-2011_01
特許番号
US07875728B2

反応ノート

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