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Acetic Acid → (R)-3-(6-Bromo-3-fluoro-pyridin-2-yl)-2,2-difluoro-3-((R)-2-methyl-propane-2-sulfinylamino)-butyric acid ethyl ester

HRID 1752457
ノート
印刷プレビュー

反応式

HRID 1752457 の反応式
[F-].[K+].[CH2:3]([O:5][C:6](=[O:34])[C:7]([F:33])([F:32])[C@@:8]([C:17]1[C:22]([F:23])=[C:21]([Si](CC)(CC)CC)[CH:20]=[C:19]([Br:31])[N:18]=1)([NH:10][S@@:11]([C:13]([CH3:16])([CH3:15])[CH3:14])=[O:12])[CH3:9])[CH3:4].C(O)(=O)C.CN(C=O)C>C1COCC1.C(OCC)(=O)C>[CH2:3]([O:5][C:6](=[O:34])[C:7]([F:32])([F:33])[C@@:8]([C:17]1[C:22]([F:23])=[CH:21][CH:20]=[C:19]([Br:31])[N:18]=1)([NH:10][S@@:11]([C:13]([CH3:16])([CH3:14])[CH3:15])=[O:12])[CH3:9])[CH3:4]
参加物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 176Acetic AcidHCID 6228DimethylformamideHCID 522689Potassium FluorideHCID 86689143(R)-3-(6-bromo-3-fluoro-4-triethylsilanyl-pyridin-2-yl)-2,2-difluoro-3-((R)-2-methyl-propane-2-sulfinylamino)-butyric acid ethyl ester

生成物 1

HCID 86689142(R)-3-(6-Bromo-3-fluoro-pyridin-2-yl)-2,2-difluoro-3-((R)-2-methyl-propane-2-sulfinylamino)-butyric acid ethyl ester
収率 88%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Freshly ground KF (195 mg, 3.36 mmol) was added to a solution of (R)-3-(6-bromo-3-fluoro-4-triethylsilanyl-pyridin-2-yl)-2,2-difluoro-3-((R)-2-methyl-propane-2-sulfinylamino)-butyric acid ethyl ester (940 mg, 1.68 mmol) and acetic acid (0.192 ml, 3.36 mmol) in THF (7 ml). DMF (7 ml) was added and the suspension was stirred at rt. After 2 h the reaction mixture was diluted with ethyl acetate and washed with sat. sodium bicarbonate solution and brine, dried over sodium sulfate, filtered and evaporated. The crude product (733 mg) was chromatographed over silica gel (cyclohexane/ethyl acetate 7:3) to give the title compound as a slightly yellow oil. 664 mg (88% yield).

後処理

  1. washwashed with sat. sodium bicarbonate solution and brine
  2. dry with materialdried over sodium sulfate
  3. filtrationfiltered
  4. customevaporated
  5. customThe crude product (733 mg) was chromatographed over silica gel (cyclohexane/ethyl acetate 7:3)

出典と根拠

ORDレコード
ord-a8047e20f19b43c3910a9efe2e51bfec
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09163011B2

反応ノート

読み込み中…

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