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Triphenylphosphine → 4-chloro-3-(1-methyl-1H-pyrazol-4-yl)-1-(2-(4-methylpiperazin-1-yl)ethyl)-5-phenyl-1H-pyrazolo[3,4-c]pyridazine

HRID 588563
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반응식

HRID 588563 반응식
[Cl:1][C:2]1[C:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[N:6][N:5]=[C:4]2[NH:14][N:15]=[C:16](I)[C:3]=12.ClC1C(C2C=CC=CC=2)=NN=[C:21]2[NH:31][N:32]=[CH:33][C:20]=12.[CH3:34][N:35]1[CH2:40][CH2:39][N:38]([CH2:41][CH2:42]O)[CH2:37][CH2:36]1.N(C(OCC)=O)=N[C:46](OCC)=O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>O1CCOCC1>[Cl:1][C:2]1[C:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[N:6][N:5]=[C:4]2[N:14]([CH2:42][CH2:41][N:38]3[CH2:39][CH2:40][N:35]([CH3:34])[CH2:36][CH2:37]3)[N:15]=[C:16]([C:20]3[CH:21]=[N:31][N:32]([CH3:46])[CH:33]=3)[C:3]=12
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 2311841-(2-Hydroxyethyl)-4-methylpiperazineHCID 867172634-chloro-5-phenyl-1H-pyrazolo[3,4-c]pyridazineHCID 86717264CID 86717264

생성물 1

HCID 74220953
4-chloro-3-(1-methyl-1H-pyrazol-4-yl)-1-(2-(4-methylpiperazin-1-yl)ethyl)-5-phenyl-1H-pyrazolo[3,4-c]pyridazine

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A solution of 4-chloro-3-iodo-5-phenyl-1H-pyrazolo[3,4-c]pyridazine and 4-chloro-5-phenyl-1H-pyrazolo[3,4-c]pyridazine (9:1, 1.4 g), 2-(4-methylpiperazin-1-yl)ethanol (1.13 g, 7.8 mmol), diethyl azodicarboxylate (1.37 g, 7.8 mmol) and triphenyl phosphine (2.07 g, 7.9 mmol) in 1,4-dioxane (26 mL) was heated to 85° C. for 1 h and then cooled to room temperature and concentrated in vacuo. The residue was partially purified by column chromatography (silica gel, starting with iso-hexanes/ethyl acetate 1:0 to 0:1 and finishing with ethyl acetate/4 M NH3 in MeOH 1:0 to 9:1). The residue was purified by preparative HPLC to provide Compounds Ia, Ib, and 20.

후처리

  1. concentrationconcentrated in vacuo
  2. customThe residue was partially purified by column chromatography (silica gel, starting with iso-hexanes/ethyl acetate 1:0 to 0:1 and finishing with ethyl acetate/4 M NH3 in MeOH 1:0 to 9:1)
  3. customThe residue was purified by preparative HPLC
  4. customto provide Compounds Ia, Ib, and 20

출처 및 근거

ORD 기록
ord-a1e2d75a23b14d10a89a5c9a8ca82ca6
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09227976B2

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