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Lithium Hydroxide → N-(4-chloro-5-(trifluoromethyl)-1H-pyrrolo[2,3-b]pyridin-3-yl)-2-methoxyacetamide

HRID 408288
ノート
印刷プレビュー

反応式

HRID 408288 の反応式
[CH3:1][O:2][CH2:3][C:4](Cl)=[O:5].[Cl:7][C:8]1[C:13]([C:14]([F:17])([F:16])[F:15])=[CH:12][N:11]=[C:10]2[NH:18][CH:19]=[C:20]([NH2:21])[C:9]=12.[Li+].[OH-]>N1C=CC=CC=1.C1COCC1>[Cl:7][C:8]1[C:13]([C:14]([F:17])([F:15])[F:16])=[CH:12][N:11]=[C:10]2[NH:18][CH:19]=[C:20]([NH:21][C:4](=[O:5])[CH2:3][O:2][CH3:1])[C:9]=12
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 3

HCID 3939Lithium HydroxideHCID 96623Methoxyacetyl chlorideHCID 602053084-chloro-5-(trifluoromethyl)-1H-pyrrolo[2,3-b]pyridin-3-amine

生成物 1

HCID 60205465N-(4-chloro-5-(trifluoromethyl)-1H-pyrrolo[2,3-b]pyridin-3-yl)-2-methoxyacetamide収率 98.1%

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒
HCID 8028
Tetrahydrofuran
溶媒

反応条件

温度
0 °C

実験手順

2-Methoxyacetyl chloride (0.074 mL, 0.76 mmol) was added to a solution of 4-chloro-5-(trifluoromethyl)-1H-pyrrolo[2,3-b]pyridin-3-amine (120 mg, 0.51 mmol, Example 12, Steps A-G) in pyridine (5 mL) at 0° C. The reaction was stirred at 0° C. for 10 minutes, and the pyridine was removed in vacuo. The residue obtained was dissolved in THF (5 mL), treated with 2N LiOH (3 mL) and stirred for 20 minutes. THF was then removed under reduced pressure, and the aqueous slurry obtained was extracted with water (20 mL) and ethyl acetate (50 mL). The organic layer was separated, washed with brine, dried (Na2SO4) and concentrated in vacuo to provide N-(4-chloro-5-(trifluoromethyl)-1H-pyrrolo[2,3-b]pyridin-3-yl)-2-methoxyacetamide (154 mg, 98% yield) as a solid.

後処理

  1. customthe pyridine was removed in vacuo
  2. customThe residue obtained
  3. stirringstirred for 20 minutes
  4. customTHF was then removed under reduced pressure
  5. customthe aqueous slurry obtained
  6. extractionwas extracted with water (20 mL) and ethyl acetate (50 mL)
  7. customThe organic layer was separated
  8. washwashed with brine
  9. dry with materialdried (Na2SO4)
  10. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-c88729606f364b9981afa4904e4190b7
出典データセット
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08758830B2

反応ノート

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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