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Methyl iodide → Methyl {(8R)-8-[[(4-fluorophenyl)sulfonyl](methyl)amino]-6,7,8,9-tetrahydro-pyrido[3,2-b]indolizin-5-yl}acetate

HRID 1036635
ノート
印刷プレビュー

反応式

HRID 1036635 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][C@@H:12]2[CH2:20][CH2:19][C:18]3[N:14]([C:15]4[N:29]=[CH:28][CH:27]=[CH:26][C:16]=4[C:17]=3[CH2:21][C:22]([O:24][CH3:25])=[O:23])[CH2:13]2)(=[O:10])=[O:9])=[CH:4][CH:3]=1.CI.[C:32]([O-])(=O)C.[NH4+].C(OCC)(=O)C>CN(C=O)C>[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N:11]([CH3:32])[C@@H:12]2[CH2:20][CH2:19][C:18]3[N:14]([C:15]4[N:29]=[CH:28][CH:27]=[CH:26][C:16]=4[C:17]=3[CH2:21][C:22]([O:24][CH3:25])=[O:23])[CH2:13]2)(=[O:9])=[O:10])=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6328Methyl iodideHCID 8857Ethyl AcetateHCID 517165Ammonium AcetateHCID 86655917methyl ((8R)-8-{[(4-fluorophenyl)sulfonyl]amino}-6,7,8,9-tetrahydropyrido[3,2-b]indolizin-5-yl)acetate

生成物 1

HCID 58360206Methyl {(8R)-8-[[(4-fluorophenyl)sulfonyl](methyl)amino]-6,7,8,9-tetrahydro-pyrido[3,2-b]indolizin-5-yl}acetate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of methyl ((8R)-8-{[(4-fluorophenyl)sulfonyl]amino}-6,7,8,9-tetrahydropyrido[3,2-b]indolizin-5-yl)acetate (0.46 g, 1.1 mmol) in DMF (5.5 mL) was added at 0° C. under nitrogen 60% NaH in oil (0.04 g, 1.2 mmol, 1.1 equiv.). After a period of 10 min., methyl iodide (0.076 mL, 1.2 mmol, 1.1 equiv.) was added and the reaction mixture aged 1 h at room temperature. The reaction mixture was poured over 25% aqueous ammonium acetate solution and ethyl acetate. The organic phase was separated, dried over sodium sulfate, filtered and evaporated under reduced pressure. The residue was purified by combiflash (hexane to 100% ethyl acetate) to provide 420 mg of the title compound.

後処理

  1. waitthe reaction mixture aged 1 h at room temperature
  2. customThe organic phase was separated
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. customevaporated under reduced pressure
  6. customThe residue was purified by combiflash (hexane to 100% ethyl acetate)

出典と根拠

ORDレコード
ord-13341547a7c44864a2e19c73a31cc5a7
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08546422B2

反応ノート

読み込み中…

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