Ammonium Chloride → HCID 178509156, 화합물

HRID 255003노트

반응식

HRID 255003 반응식
[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

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 178509157HCID 178509157, 화합물HCID 178510679HCID 178510679, 화합물

생성물 1

HCID 178509156HCID 178509156, 화합물수율 51%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-e5ddff6737f6419ab336e9d6563831f0
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07875728B2

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