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1-Benzyl-4-piperidylamine → tert-Butyl 2-((1-benzylpiperidin-4-ylamino)methyl)-6-fluorophenylcarbamate

HRID 501973
ノート
印刷プレビュー

反応式

HRID 501973 の反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH:8]=O)[C:3]=1[NH:10][C:11](=[O:17])[O:12][C:13]([CH3:16])([CH3:15])[CH3:14].[NH2:18][CH:19]1[CH2:24][CH2:23][N:22]([CH2:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[CH2:21][CH2:20]1.[BH4-].[Na+]>C(O)C>[CH2:25]([N:22]1[CH2:23][CH2:24][CH:19]([NH:18][CH2:8][C:4]2[CH:5]=[CH:6][CH:7]=[C:2]([F:1])[C:3]=2[NH:10][C:11](=[O:17])[O:12][C:13]([CH3:16])([CH3:15])[CH3:14])[CH2:20][CH2:21]1)[C:26]1[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=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

5

反応物 3

HCID 4158521-Benzyl-4-piperidylamine2 回HCID 4311764Sodium borohydride2 回HCID 11506970Tert-butyl 2-fluoro-6-formylphenylcarbamate

生成物 1

HCID 59424374tert-Butyl 2-((1-benzylpiperidin-4-ylamino)methyl)-6-fluorophenylcarbamate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
0 °C

実験手順

To a solution of tert-butyl 2-fluoro-6-formylphenylcarbamate (48.0 g, 201 mmol) in ethanol (100 mL) was added 4-amino-1-benzylpiperidine (41.0 mL, 201 mmol). The solution was concentrated in vacuo, and then water was removed by twice dissolving the residue in toluene and concentrating the solution in vacuo. The resulting oil was dissolved in tetrahydrofuran (250 mL), cooled to 0° C., and treated with sodium borohydride (3.80 g, 100 mmol). The ice bath was removed and stirring continued overnight. The reaction was treated with ethanol (250 mL), an additional portion of sodium borohydride (2.00 g, 53 mmol), and an additional portion of 4-amino-1-benzylpiperidine (2.0 mL, 9.8 mmol). The resulting solution was stirred for 4 h at room temperature. The reaction was cooled to 0° C., quenched by addition of saturated ammonium chloride, filtered to remove solids, and concentrated to remove most (but not all) of the tetrahydrofuran. The reaction was extracted with diethyl ether (2×). The ethereal layer was washed with water (3×), then brine, dried over magnesium sulfate, and concentrated to give 83 g (100%) as a viscous yellow oil which was pure enough to use in the following step. Mass spec.: 414.51 (MH)+.

後処理

  1. concentrationThe solution was concentrated in vacuo
  2. customwater was removed
  3. dissolutionby twice dissolving the residue in toluene
  4. concentrationconcentrating the solution in vacuo
  5. dissolutionThe resulting oil was dissolved in tetrahydrofuran (250 mL)
  6. customThe ice bath was removed
  7. additionThe reaction was treated with ethanol (250 mL)
  8. stirringThe resulting solution was stirred for 4 h at room temperature
  9. temperatureThe reaction was cooled to 0° C.
  10. customquenched by addition of saturated ammonium chloride
  11. filtrationfiltered
  12. customto remove solids
  13. concentrationconcentrated
  14. customto remove most (but not all) of the tetrahydrofuran
  15. extractionThe reaction was extracted with diethyl ether (2×)
  16. washThe ethereal layer was washed with water (3×)
  17. dry with materialbrine, dried over magnesium sulfate
  18. concentrationconcentrated
  19. customto give 83 g (100%) as a viscous yellow oil which

出典と根拠

ORDレコード
ord-1bb4baaa633a43dcb30ca5d6c57b3e18
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07772244B2

反応ノート

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