ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Water → 1-(1-Methylethyl)-N-[6-(2-oxo-2,3-dihydro-1,3-benzoxazol-7-yl)-1H-indazol-4-yl]-1H-pyrazole-5-carboxamide

HRID 244745
ノート
印刷プレビュー

反応式

HRID 244745 の反応式
P([O-])([O-])([O-])=O.[K+].[K+].[K+].Br[C:10]1[C:18]2[O:17][C:16](=[O:19])[NH:15][C:14]=2[CH:13]=[CH:12][CH:11]=1.[CH3:20][CH:21]([N:23]1[C:27]([C:28]([NH:30][C:31]2[C:32]3[C:36]([CH:37]=[C:38](B4OC(C)(C)CC(C)(C)O4)[CH:39]=2)=[N:35][N:34](C2CCCCO2)[CH:33]=3)=[O:29])=[CH:26][CH:25]=[N:24]1)[CH3:22].O>O1CCOCC1.CO>[CH3:22][CH:21]([N:23]1[C:27]([C:28]([NH:30][C:31]2[CH:39]=[C:38]([C:10]3[C:18]4[O:17][C:16](=[O:19])[NH:15][C:14]=4[CH:13]=[CH:12][CH:11]=3)[CH:37]=[C:36]3[C:32]=2[CH:33]=[N:34][NH:35]3)=[O:29])=[CH:26][CH:25]=[N:24]1)[CH3:20]
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

7

反応物 4

HCID 962WaterHCID 62657Potassium Phosphate, TribasicHCID 115575587-Bromobenzo[d]oxazol-2(3H)-oneHCID 582557371-(1-Methylethyl)-N-[2-(tetrahydro-2H-pyran-2-yl)-6-(4,4,6,6-tetramethyl-1,3,2-dioxaborinan-2-yl)-2H-indazol-4-yl]-1H-pyrazole-5-carboxamide

生成物 1

HCID 583564261-(1-Methylethyl)-N-[6-(2-oxo-2,3-dihydro-1,3-benzoxazol-7-yl)-1H-indazol-4-yl]-1H-pyrazole-5-carboxamide

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
120 °C

実験手順

A microwave vial was charged with Solvias catalyst (8 mg), tripotassium phosphate (90 mg) and 7-bromo-1,3-benzoxazol-2(3H)-one (from prep. such as US2006/0122189A1, 33 mg). 1-(1-Methylethyl)-N-[2-(tetrahydro-2H-pyran-2-yl)-6-(4,4,6,6-tetramethyl-1,3,2-dioxaborinan-2-yl)-2H-indazol-4-yl]-1H-pyrazole-5-carboxamide (70 mg) in 1,4-dioxane (0.5 ml) was added followed by water (0.1 ml). The reaction was heated under microwave irradiation at 120° C. for 10 min. The reaction was passed through a silica cartridge preconditioned with methanol, washing with methanol, then dried under a stream of nitrogen. The residue was subjected to a DCM/water wash and then dried under a stream of nitrogen. The residue was dissolved in DMSO:methanol (1 ml, 1:1, v/v) and purified by MDAP (method A). Appropriate fractions were evaporated under a stream of nitrogen. The residues were dissolved in a minimum amount of methanol and combined. A few drops of 2M HCl (aq) were added and the reaction was left to stand at room temperature. The reaction was then evaporated under a stream of nitrogen, passed through an aminopropyl cartridge and dried to give title compound, 10 mg.

後処理

  1. washwashing with methanol
  2. customdried under a stream of nitrogen
  3. washwash
  4. customdried under a stream of nitrogen
  5. dissolutionThe residue was dissolved in DMSO
  6. custommethanol (1 ml, 1:1, v/v) and purified by MDAP (method A)
  7. customAppropriate fractions were evaporated under a stream of nitrogen
  8. dissolutionThe residues were dissolved in a minimum amount of methanol
  9. additionA few drops of 2M HCl (aq) were added
  10. waitthe reaction was left
  11. customto stand at room temperature
  12. customThe reaction was then evaporated under a stream of nitrogen
  13. customdried

出典と根拠

ORDレコード
ord-befc2fce4ee8422a8bd10e6b95c4cda3
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08658635B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート