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 → 3-{[2-Fluoro-1-(fluoromethyl)ethyl]oxy}-5-[(9-fluoro-4-methyl-5-oxo-2,3,4,5-tetrahydro-1,4-benzoxazepin-8-yl)oxy]-n-(1-methyl-1h-pyrazol-3-yl)benzamide

HRID 548682
ノート
印刷プレビュー

反応式

HRID 548682 の反応式
[F:1][CH2:2][CH:3]([O:6][C:7]1[CH:8]=[C:9]([CH:19]=[C:20]([OH:22])[CH:21]=1)[C:10]([NH:12][C:13]1[CH:17]=[CH:16][N:15]([CH3:18])[N:14]=1)=[O:11])[CH2:4][F:5].CC([Si](C)(C)[O:28][CH2:29][CH2:30][N:31]([CH3:43])[C:32](=[O:42])[C:33]1[CH:38]=[CH:37][C:36](F)=[C:35]([F:40])[C:34]=1F)(C)C.C(=O)([O-])[O-].[K+].[K+].O>CC(N(C)C)=O>[F:5][CH2:4][CH:3]([O:6][C:7]1[CH:8]=[C:9]([CH:19]=[C:20]([O:22][C:36]2[CH:37]=[CH:38][C:33]3[C:32](=[O:42])[N:31]([CH3:43])[CH2:30][CH2:29][O:28][C:34]=3[C:35]=2[F:40])[CH:21]=1)[C:10]([NH:12][C:13]1[CH:17]=[CH:16][N:15]([CH3:18])[N:14]=1)=[O:11])[CH2:2][F:1]
参加物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 962WaterHCID 11430Potassium CarbonateHCID 57663171N-(2-{[(1,1-Dimethylethyl)(dimethyl)silyl]oxy}ethyl)-2,3,4-trifluoro-N-methylbenzamideHCID 591271643-{[2-fluoro-1-(fluoromethyl)ethyl]oxy}-5-hydroxy-N-(1-methyl-1H-pyrazol-3-yl)benzamide

生成物 1

HCID 159494053-{[2-Fluoro-1-(fluoromethyl)ethyl]oxy}-5-[(9-fluoro-4-methyl-5-oxo-2,3,4,5-tetrahydro-1,4-benzoxazepin-8-yl)oxy]-n-(1-methyl-1h-pyrazol-3-yl)benzamide
収率 3.1%

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

A solution of 3-{[2-fluoro-1-(fluoromethyl)ethyl]oxy}-5-hydroxy-N-(1-methyl-1H-pyrazol-3-yl)benzamide (100 mg, 0.32 mmol), N-(2-{[(1,1-dimethylethyl)(dimethyl)silyl]oxy}ethyl)-2,3,4-trifluoro-N-methylbenzamide (112 mg, 0.32 mmol) and potassium carbonate (89 mg, 0.64 mmol) in DMA (2 mL) was heated in a microwave reactor for 2 hours. Water (20 mL) was added and the solution extracted with ethyl acetate. The ethyl acetate layer was washed with brine (20 mL), dried (MgSO4) and evaporated to a residue which was taken up in DCM (10 mL) and TFA (5 drops) added. The mixture was stirred at RT for 2 hours. The solvent was evaporated to a residue, which was chromatographed by preparative HPLC on C18 reversed phase, eluting with 5-95% acetonitrile (+0.2% TFA) in water (+0.2% TFA), to give the required product (5 mg).

後処理

  1. extractionthe solution extracted with ethyl acetate
  2. washThe ethyl acetate layer was washed with brine (20 mL)
  3. dry with materialdried (MgSO4)
  4. customevaporated to a residue which
  5. additionTFA (5 drops) added
  6. customThe solvent was evaporated to a residue, which
  7. customwas chromatographed by preparative HPLC on C18 reversed phase
  8. washeluting with 5-95% acetonitrile (+0.2% TFA) in water (+0.2% TFA)

出典と根拠

ORDレコード
ord-5c476d9a34f5470b9fd75eff910976dd
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07943607B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート