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Methanol → HCID 58190476、化合物

HRID 1892410
ノート
印刷プレビュー

反応式

HRID 1892410 の反応式
O=[C:2]1[C:10]2C(=CC=CC=2)C(=O)[N:3]1[O:12][CH2:13][C:14]([NH2:16])=[O:15].O.NN.CO.[N:22]1[C:31]2[C:26](=[CH:27][C:28]([CH2:32][C:33]3[N:37]4[N:38]=[C:39](C(=O)C)[CH:40]=[CH:41][C:36]4=[N:35][N:34]=3)=[CH:29][CH:30]=2)[CH:25]=[CH:24][CH:23]=1>C(O)(=O)C>[N:22]1[C:31]2[C:26](=[CH:27][C:28]([CH2:32][C:33]3[N:37]4[N:38]=[C:39](/[C:2](=[N:3]/[O:12][CH2:13][C:14]([NH2:16])=[O:15])/[CH3:10])[CH:40]=[CH:41][C:36]4=[N:35][N:34]=3)=[CH:29][CH:30]=2)[CH:25]=[CH:24][CH:23]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 887MethanolHCID 24654Hydrazine hydrate (1:1)HCID 140744182-[(1,3-Dioxo-1,3-dihydro-2H-isoindol-2-yl)oxy]acetamide2 回HCID 581904611-(3-(Quinolin-6-ylmethyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)ethanone

生成物 1

HCID 58190476HCID 58190476、化合物

試薬・触媒・溶媒 1

HCID 176
Acetic Acid
溶媒

反応条件

温度
95 °C

実験手順

A microwave tube was charged with 2-(1,3-dioxoisoindolin-2-yloxy)acetamide (intermediate V) (166 mg, 0.76 mmol), hydrazine monohydrate (34.4 mg, 0.69 mmol) and 2 mL of methanol. It was heated at 95° C. for 12 h under microwave irradiation. After cooling, solid was removed by filtration and the solution was concentrated under reduced pressure. The residue was diluted with methanol, then 1-(3-(quinolin-6-ylmethyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)ethanone (41.2) (32 mg, 0.105 mmol) and 0.3 mL of acetic acid were added and the mixture was stirred at 40° C. overnight. After concentration, the residue was purified by prep-HPLC to afford the title compound. 1H-NMR (400 MHz, DMSO-d6) δ ppm 8.86 (dd, 1H), 8.33-8.27 (m, 2H), 7.98-7.95 (m, 2H), 7.78 (dd, 1H), 7.69 (d, 1H), 7.50 (dd, 1H), 7.31 (d, 2H), 4.77 (s, 2H), 4.63 (s, 2H), 2.32 (s, 3H). LCMS (method A): [MH]+=376, tR=4.02 min.

後処理

  1. temperatureAfter cooling
  2. customsolid was removed by filtration
  3. concentrationthe solution was concentrated under reduced pressure
  4. additionThe residue was diluted with methanol
  5. concentrationAfter concentration
  6. customthe residue was purified by prep-HPLC

出典と根拠

ORDレコード
ord-2f8cfdcbaaf74db48974029e9110f9d2
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08507676B2

反応ノート

読み込み中…

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