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Potassium tert-butoxide → HCID 90093877、化合物

HRID 1753073
ノート
印刷プレビュー

反応式

HRID 1753073 の反応式
[CH3:1][O:2][C:3](=[O:17])[CH:4]([N:6]1[C:14]2[C:13]([F:15])=[CH:12][N:11]=[CH:10][C:9]=2[C:8]([I:16])=[CH:7]1)[CH3:5].[CH3:18]C(C)([O-])C.[K+]>C1COCC1>[CH3:1][O:2][C:3](=[O:17])[C:4]([N:6]1[C:14]2[C:13]([F:15])=[CH:12][N:11]=[CH:10][C:9]=2[C:8]([I:16])=[CH:7]1)([CH3:18])[CH3:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 23665647Potassium tert-butoxideHCID 90093829HCID 90093829、化合物

生成物 1

HCID 90093877HCID 90093877、化合物収率 78.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred solution of 2-(7-fluoro-3-iodo-pyrrolo[3,2-c]pyridin-1-yl)-propionic acid methyl ester (8 g, 22.98 mmol) in dry THF (80 mL) was added Mel (1.85 mL, 29.87 mmol) and the flask was placed in a water bath. Potassium tert-butoxide (1M in THF, 29.87 mL, 29.87 mmol) was added over 10 minutes and the mixture was stirred for an additional 10 minutes. Then reaction was quenched with water and few drops of 0.2M HCl and then diluted with EtOAc. The organic layer was washed with water, brine, dried over sodium sulphate and evaporated in vacuo. The crude material was purified by silica gel column chromatography eluting with 0-20% EtOAc in Hexane to afford the title compound as light yellow solid (78%, 6.5 g).

後処理

  1. customthe flask was placed in a water bath
  2. customThen reaction
  3. customwas quenched with water and few drops of 0.2M HCl
  4. additiondiluted with EtOAc
  5. washThe organic layer was washed with water, brine
  6. dry with materialdried over sodium sulphate
  7. customevaporated in vacuo
  8. customThe crude material was purified by silica gel column chromatography
  9. washeluting with 0-20% EtOAc in Hexane

出典と根拠

ORDレコード
ord-f9ced9c313524f8589b1c4728084a1fc
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09163021B2

反応ノート

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