Water → 1-(4-acetylphenyl)-8-{[(2-chloropyridin-3-yl)carbonyl]amino}-4,5-dihydro-1H-benzo[g]indazole-3-carboxamide

HRID 968132ノート

反応式

HRID 968132 の反応式
[Cl:1][C:2]1[C:7]([C:8]([NH:10][C:11]2[CH:34]=[CH:33][C:14]3[CH2:15][CH2:16][C:17]4[C:18]([C:30]([NH2:32])=[O:31])=[N:19][N:20]([C:22]5[CH:27]=[CH:26][C:25]([C:28]#[CH:29])=[CH:24][CH:23]=5)[C:21]=4[C:13]=3[CH:12]=2)=[O:9])=[CH:6][CH:5]=[CH:4][N:3]=1.O.[OH:36]S(C(F)(F)F)(=O)=O.C([O-])(O)=O.[Na+]>O1CCOCC1>[C:28]([C:25]1[CH:26]=[CH:27][C:22]([N:20]2[C:21]3[C:13]4[CH:12]=[C:11]([NH:10][C:8]([C:7]5[C:2]([Cl:1])=[N:3][CH:4]=[CH:5][CH:6]=5)=[O:9])[CH:34]=[CH:33][C:14]=4[CH2:15][CH2:16][C:17]=3[C:18]([C:30]([NH2:32])=[O:31])=[N:19]2)=[CH:23][CH:24]=1)(=[O:36])[CH3:29]

参加物

6

反応物 4

HCID 962WaterHCID 62406Trifluoromethanesulfonic acidHCID 516892Sodium BicarbonateHCID 222915468-{[(2-chloropyridin-3-yl)carbonyl]amino}-1-(4-ethynylphenyl)-4,5-dihydro-1H-benzo[g]indazole-3-carboxamide

生成物 1

HCID 222915781-(4-acetylphenyl)-8-{[(2-chloropyridin-3-yl)carbonyl]amino}-4,5-dihydro-1H-benzo[g]indazole-3-carboxamide

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

A mixture of 8-{[(2-chloropyridin-3-yl)carbonyl]amino}-1-(4-ethynylphenyl)-4,5-dihydro-1H-benzo[g]indazole-3-carboxamide (442 mg, 1.2 mmol), water (65 mg, 3.6 mmol), and triflic acid (270 mg, 1.8 mmol) in dioxane (10 mL) was heated to 100° C. for 18 h. The mixture was cooled to RT, aqueous NaHCO3 was added, and filtered. The product was washed with water and ether, and dried. This gave product (293 mg, 67%). 1H NMR was consistent with its structure.

後処理

  1. temperatureThe mixture was cooled to RT
  2. filtrationfiltered
  3. washThe product was washed with water and ether
  4. customdried

出典と根拠

ORDレコード
ord-f0cf18bd920b45d3b141dc7dd8c1146b
出典データセット
uspto-grants-2005_10
特許番号
US06956052B2

反応ノート

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