Triphenylphosphine → 7-(Pyridin-4-yl)-5-[2-(quinolin-2-yl)ethyl]thieno[2,3-d]pyridazin-4(5H)-one

HRID 920903ノート

反応式

HRID 920903 の反応式
[N:1]1[CH:6]=[CH:5][C:4]([C:7]2[C:8]3[S:16][CH:15]=[CH:14][C:9]=3[C:10](=[O:13])[NH:11][N:12]=2)=[CH:3][CH:2]=1.[N:17]1[C:26]2[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=2)[CH:20]=[CH:19][C:18]=1[CH2:27][CH2:28]O.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.CCOC(/N=N/C(OCC)=O)=O>C(Cl)Cl>[N:1]1[CH:2]=[CH:3][C:4]([C:7]2[C:8]3[S:16][CH:15]=[CH:14][C:9]=3[C:10](=[O:13])[N:11]([CH2:28][CH2:27][C:18]3[CH:19]=[CH:20][C:21]4[C:26](=[CH:25][CH:24]=[CH:23][CH:22]=4)[N:17]=3)[N:12]=2)=[CH:5][CH:6]=1

参加物

6

反応物 4

HCID 11776TriphenylphosphineHCID 705322-QuinolineethanolHCID 5462977Diethyl azodicarboxylateHCID 866831187-(pyridin-4-yl)thieno[3,2-d]pyridazin-4(5H)-one

生成物 1

HCID 715574477-(Pyridin-4-yl)-5-[2-(quinolin-2-yl)ethyl]thieno[2,3-d]pyridazin-4(5H)-one収率 11.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 7-(pyridin-4-yl)thieno[3,2-d]pyridazin-4(5H)-one (100 mg, 0.44 mmol) from example 2.3, 2-quinolin-2-yl-ethanol from example a1 (83 mg, 0.48 mmol) and PPh3 (343 mg, 1.31 mmol) in DCM (10 mL), DEAD (228 mg, 1.31 mmol) was added dropwise. The mixture stirred at room temperature for 3 h, concentrated and the purified by Prep-HPLC to give the title compound as a white solid (20 mg, 11.8% yield).

後処理

  1. concentrationconcentrated
  2. customthe purified by Prep-HPLC

出典と根拠

ORDレコード
ord-c7921e9f87814867b47e2b0cd1163bce
出典データセット
uspto-grants-2016_03
特許番号
US09273068B2

反応ノート

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