Ammonium Chloride → HCID 178509156、化合物

HRID 2095169ノート

反応式

HRID 2095169 の反応式
[NH2:1][C:2]1[C:3](=[N:16][NH:17][C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([F:24])[CH:19]=2)[C:4]([CH2:7][NH:8][C:9](=[O:15])[CH2:10][CH2:11][C:12]([OH:14])=[O:13])=[N:5][N:6]=1.NCC1C(=NNC2C=CC=C(F)C=2)C(N)=NN=1.[Cl-].[NH4+]>C(OCC)(=O)C>[NH2:1][C:2]1[C:3](=[N:16][NH:17][C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([F:24])[CH:19]=2)[C:4]([CH2:7][NH:8][C:9]([CH:10]=[CH:11][C:12]([OH:14])=[O:13])=[O:15])=[N:5][N:6]=1

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 178509157HCID 178509157、化合物HCID 178510679HCID 178510679、化合物

生成物 1

HCID 178509156HCID 178509156、化合物収率 51%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

In a similar manner, N-{5-amino-4-[(3-fluorophenyl)hydrazono]-4H-pyrazol-3-ylmethyl}succinamic acid was prepared by reacting 5-aminomethyl-4-[(3-fluorophenyl)hydrazono]-4H-pyrazol-3-ylamine (60 mg, 0.25 mmole) with succinic anhydide (40 mg, 0.4 mmole). The reaction was worked up by the addition of aqueous ammonium chloride solution and ethyl acetate. The crude material was purified by preparative TLC (CH2Cl2:CH3OH:H2O:HOAc=210:21:1.6:0.8) to yield 45 mg (51%) of the title compound as a yellow powder. MS (m/z, ES−): 333 (M−1, 42%); 1H NMR (ppm, 300 MHz, DMSO-d6) δ 8.23 (br s, 1H), 7.35-7.63 (m, 3H), 6.83-7.20 (m, 3H), 4.42 (s, 2H), 2.33 (m, 4H).

後処理

  1. customThe crude material was purified by preparative TLC (CH2Cl2:CH3OH:H2O:HOAc=210:21:1.6:0.8)

出典と根拠

ORDレコード
ord-91be3a0e06fb45c6b295644ae15826ce
出典データセット
uspto-grants-2013_05
特許番号
US08445694B2

反応ノート

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