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Aniline → ethyl 2-[3-[(N-[(3R)-quinuclidin-3-yl]oxycarbonyl-anilino)methyl]phenyl]acetate

HRID 1497989
ノート
印刷プレビュー

反応式

HRID 1497989 の反応式
Br[CH2:2][C:3]1[CH:4]=[C:5]([CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])[CH:6]=[CH:7][CH:8]=1.[NH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.C(=O)([O-])[O-].[K+].[K+].Cl.[C:29](Cl)(=[O:39])[O:30][C@@H:31]1[CH:36]2[CH2:37][CH2:38][N:33]([CH2:34][CH2:35]2)[CH2:32]1>>[N:33]12[CH2:38][CH2:37][CH:36]([CH2:35][CH2:34]1)[C@@H:31]([O:30][C:29]([N:15]([CH2:2][C:3]1[CH:4]=[C:5]([CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])[CH:6]=[CH:7][CH:8]=1)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)=[O:39])[CH2:32]2
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

5

反応物 4

HCID 6115AnilineHCID 11430Potassium CarbonateHCID 10563066Ethyl 2-(3-(bromomethyl)phenyl)acetateHCID 86676896(3R)-1-azabicyclo[2.2.2]octan-3-yl carbonochloridate hydrochloride

生成物 1

HCID 86720711ethyl 2-[3-[(N-[(3R)-quinuclidin-3-yl]oxycarbonyl-anilino)methyl]phenyl]acetate収率 35.4%

反応条件

温度
90 °C

実験手順

A mixture of ethyl 2-[3-(bromomethyl)phenyl]acetate (600 mg, 2.33 mmol), aniline (202 mg, 2.21 mmol) and potassium carbonate (420 mg, 3.04 mmol) in 1V, N-dimethylformamide (15 mL) was heated to 90° C. for 18 hours. After cooling to room temperature, the reaction was filtered and the solvent was removed in vacuo. The residue was taken up in ethyl acetate and washed with brine (3×20 mL). The organic phase was passed through a hydrophobic fit and the solvent was removed in vacuo. The crude material was dissolved in acetonitrile (5 mL), and (R)-quinuclidin-3-yl carbonochloridate hydrochloride (530 mg, 2.35 mmol) was added. The resulting mixture was heated to 100° C. for 30 minutes under microwave irradiation. The solvent was removed in vacuo, then the residue was partitioned between ethyl acetate and saturated aqueous sodium bicarbonate solution. The organic layer was washed with brine, passed through a hydrophobic fit and the solvent was removed in vacuo. The residue was purified by silica gel column chromatography eluting sequentially with ethyl acetate, 10% methanol in ethyl acetate and 10% 7N methanolic ammonia in ethyl acetate to afford the title compound as a yellow solid (331 mg, 35%).

後処理

  1. temperatureAfter cooling to room temperature
  2. filtrationthe reaction was filtered
  3. customthe solvent was removed in vacuo
  4. washwashed with brine (3×20 mL)
  5. customthe solvent was removed in vacuo
  6. dissolutionThe crude material was dissolved in acetonitrile (5 mL)
  7. temperatureThe resulting mixture was heated to 100° C. for 30 minutes under microwave irradiation
  8. customThe solvent was removed in vacuo
  9. customthe residue was partitioned between ethyl acetate and saturated aqueous sodium bicarbonate solution
  10. washThe organic layer was washed with brine
  11. customthe solvent was removed in vacuo
  12. customThe residue was purified by silica gel column chromatography
  13. washeluting sequentially with ethyl acetate, 10% methanol in ethyl acetate and 10% 7N methanolic ammonia in ethyl acetate

出典と根拠

ORDレコード
ord-381900e37c6248fa9f968acd878e59b5
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09199980B2

反応ノート

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