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Trifluoroacetic anhydride → Bisegliptin

HRID 606731
ノート
印刷プレビュー

反応式

HRID 606731 の反応式
FC(F)(F)C(OC(=O)C(F)(F)F)=O.[CH2:14]([O:16][C:17]([C:19]12[CH2:26][CH2:25][C:22]([NH:27][CH2:28][C:29]([N:31]3[CH2:35][C@@H:34]([F:36])[CH2:33][C@H:32]3[C:37]([NH2:39])=O)=[O:30])([CH2:23][CH2:24]1)[CH2:21][CH2:20]2)=[O:18])[CH3:15].C(=O)(O)[O-].[Na+]>O1CCCC1>[CH2:14]([O:16][C:17]([C:19]12[CH2:26][CH2:25][C:22]([NH:27][CH2:28][C:29]([N:31]3[CH2:35][C@@H:34]([F:36])[CH2:33][C@H:32]3[C:37]#[N:39])=[O:30])([CH2:23][CH2:24]1)[CH2:21][CH2:20]2)=[O:18])[CH3:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 9845Trifluoroacetic anhydride2 回HCID 516892Sodium BicarbonateHCID 46854534(2S,4S)-1-[2-[(4-ethoxycarbonylbicyclo[2.2.2]oct-1-yl)amino]acetyl]-4-fluoropyrrolidine-2-carboxamide

生成物 1

HCID 11688894Bisegliptin収率 67%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Trifluoroacetic anhydride (80 μL) was added to a solution of (2S,4S)-1-[2-[(4-ethoxycarbonylbicyclo[2.2.2]oct-1-yl)amino]ac etyl]-4-fluoropyrrolidine-2-carboxamide (100 mg) in tetrahydrofuran (1 mL). The mixture was stirred at room temperature for 2 hours and then at 40° C. for 1.5 hours. Subsequently, additional trifluoroacetic anhydride (40 μL) was added and the mixture was further stirred for 30 minutes. A saturated aqueous sodium bicarbonate solution (5 mL) was then added and the reaction mixture was extracted with ethyl acetate (2×10 mL). The ethyl acetate extracts were combined, washed with saturated brine (5 mL), dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The resulting residue was purified on an aminated silica gel column (eluant=ethyl acetate:methanol=30:1) to give (2S,4S)-1-[2-[(4-ethoxycarbonylbicyclo[2.2.2]oct-1-yl)amino]ac etyl]-4-fluoropyrrolidine-2-carbonitrile as a colorless solid (63.7 mg, 67% yield). This compound was identical to the compound obtained in Example 7.

後処理

  1. waitat 40° C. for 1.5 hours
  2. stirringthe mixture was further stirred for 30 minutes
  3. extractionthe reaction mixture was extracted with ethyl acetate (2×10 mL)
  4. washwashed with saturated brine (5 mL)
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe resulting residue was purified on an aminated silica gel column (eluant=ethyl acetate:methanol=30:1)

出典と根拠

ORDレコード
ord-9f7ece6d8e6d43e9a461493dd80fc73c
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07915427B2

反応ノート

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