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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
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Water → HCID 21931732、化合物

HRID 2209283
ノート
印刷プレビュー

反応式

HRID 2209283 の反応式
[Cl:1][C:2]1[N:7]=C2N[C:9](=O)[CH2:10][C:5]2=[CH:4][CH:3]=1.[H-].[Na+].I[CH3:15].O.[CH3:17][N:18]([CH:20]=[O:21])[CH3:19]>[Cl-].[Na+].O.CCOC(C)=O>[Cl:1][C:2]1[N:7]=[C:17]2[N:18]([CH3:19])[C:20](=[O:21])[C:10]([CH3:9])([CH3:15])[C:5]2=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 962WaterHCID 6228Dimethylformamide2 回HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 219070476-Chloro-1,3-dihydro-2H-pyrrolo[2,3-b]pyridin-2-one

生成物 1

HCID 21931732HCID 21931732、化合物

試薬・触媒・溶媒 2

HCID 8857
Ethyl Acetate
溶媒
HCID 57417360Sodium chloride; water溶媒

実験手順

To a solution of 6-chloro-1H-pyrrolo[2,3-b]pyridin-2(3H)-one (50 mg, 0.30 mmol) in DMF (1 mL) at 0° C. was added NaH (48 mg, 1.2 mmol, 60%), and the reaction was stirred for 5 minutes. Iodomethane (210 mg, 1.5 mmol) was added and the reaction became a thick slurry. DMF (0.5 mL) was added and the reaction was stirred at room temperature for 90 minutes. Water, EtOAc, and brine were added, the layers were separated and the organic layer was washed with brine. The organics were dried over MgSO4, filtered and concentrated to afford 6-chloro-1,3,3-trimethyl-1H-pyrrolo[2,3-b]pyridin-2(3H)-one 7.28 which was used without further purification. LCMS-ESI+ (m/z): [M+H]+ calcd for C10H12ClN2O: 211.1; found: 211.0.

後処理

  1. stirringthe reaction was stirred at room temperature for 90 minutes
  2. customthe layers were separated
  3. washthe organic layer was washed with brine
  4. dry with materialThe organics were dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-c88d4d85d3904d1086c79f9e11e9607f
出典データセット
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09376441B2

反応ノート

読み込み中…

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