ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
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
  1. ホーム
  2. /反応

Triethylamine → Methyl (R)-3-(N-Cyclobutyl-N-isopropylamino)-8-fluoro-3,4-dihydro-2H-1-benzopyran-5-carboxylate

HRID 1738322
ノート
印刷プレビュー

反応式

HRID 1738322 の反応式
[CH:1]1([N:5]([C@@H:9]2[CH2:14][C:13]3[C:15](OS(C(F)(F)F)(=O)=O)=[CH:16][CH:17]=[C:18]([F:19])[C:12]=3[O:11][CH2:10]2)[CH:6]([CH3:8])[CH3:7])[CH2:4][CH2:3][CH2:2]1.[C]=O.C1(P(C2C=CC=CC=2)CCCP(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(N(CC)CC)C.CN([CH:69]=[O:70])C.[CH3:71][OH:72]>C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[CH:1]1([N:5]([C@@H:9]2[CH2:14][C:13]3=[C:15]([C:71]([O:70][CH3:69])=[O:72])[CH:16]=[CH:17][C:18]([F:19])=[C:12]3[O:11][CH2:10]2)[CH:6]([CH3:8])[CH3:7])[CH2:4][CH2:3][CH2:2]1
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

7

反応物 5

HCID 8471TriethylamineHCID 812191,3-Bis(diphenylphosphino)propaneHCID 21901440N,N-dimethylformamide methanolHCID 54082177(R)-3-(N-Cyclobutyl-N-isopropylamino)-8-fluoro-5-trifluoromethylsulfonyloxy-3,4-dihydro-2H-1-benzopyranHCID 178418416HCID 178418416、化合物

生成物 1

HCID 53695439
Methyl (R)-3-(N-Cyclobutyl-N-isopropylamino)-8-fluoro-3,4-dihydro-2H-1-benzopyran-5-carboxylate
収率 92%

試薬・触媒・溶媒 1

HCID 167845palladium(II) acetate触媒

反応条件

温度
70 °C

実験手順

(R)-3-(N-Cyclobutyl-N-isopropylamino)-8-fluoro-5-trifluoromethylsulfonyloxy-3,4-dihydro-2H-1-benzopyran (1.65 g, 4.01 mmol) was dissolved in a solution of DMF/methanol (6:2, 30 mL) and then degassed followed by the inlet of carbon monoxide (×3). With a slight positive pressure of carbon monoxide, palladium(II)-acetate (30 mg), 1,3-bis(diphenylphosphino)propane (55 mg) and triethylamine (1.25 mL, 8.8 mmol) were added and the reaction mixture was degassed and subjected to carbon monoxide once again. The reaction was heated to 70° C. under carbon monoxide atmosphere with vigorous stirring for 6 h. The reaction was allowed to cool and the solvent was removed in vacuo. The remains were taken into a 2M solution of NH3 and then extracted, twice, with diethyl ether. The combined ether portions were dried (MgSO4), filtered, and the solvent removed in vacuo to give the crude residue. Chromatography on silica (eluent: 8% ethyl acetate/hexane) gave 1.18 mg (92% yield) of the title compound as a clear oil. [α]21D =-139.1° (C=0.1; CHCl3). GC-MS (70 eV) M=321 (3%).

後処理

  1. customdegassed
  2. customthe reaction mixture was degassed
  3. temperatureto cool
  4. customthe solvent was removed in vacuo
  5. extractionextracted
  6. dry with materialThe combined ether portions were dried (MgSO4)
  7. filtrationfiltered
  8. customthe solvent removed in vacuo
  9. customto give the crude residue

出典と根拠

ORDレコード
ord-47739388784340e198437b62b867618a
出典データセット
uspto-grants-1999_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05962514

反応ノート

読み込み中…

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