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Benzylamine → tert-Butyl 4-(benzylamino)-3,3-difluoropiperidine-1-carboxylate

HRID 2280374
ノート
印刷プレビュー

反応式

HRID 2280374 の反応式
[F:1][C:2]1([F:16])[C:7](=O)[CH2:6][CH2:5][N:4]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:3]1.[CH2:17]([NH2:24])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C([O-])([O-])=O.[Na+].[Na+]>C(Cl)Cl>[CH2:17]([NH:24][CH:7]1[CH2:6][CH2:5][N:4]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:3][C:2]1([F:16])[F:1])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=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 7504BenzylamineHCID 10340Sodium CarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 56776981tert-Butyl 3,3-difluoro-4-oxopiperidine-1-carboxylate

生成物 1

HCID 66710726tert-Butyl 4-(benzylamino)-3,3-difluoropiperidine-1-carboxylate

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

To a solution of tert-butyl 3,3-difluoro-4-oxopiperidine-1-carboxylate (0.250 g, 1.06 mmol) in CH2Cl2 (4.5 mL) was added benzylamine (0.13 mL, 1.17 mmol) and sodium triacetoxyborohydride (0.356 g, 1.59 mmol) and the solution was stirred at rt for 22 h. The reaction mixture was treated with sat. aq. Na2CO3 and extracted with EA (3×50 mL). The combined organic extracts were dried over MgSO4, filtered, and the solvent removed under reduced pressure. The residue was purified by FC (Heptane/EA, 1:1) to give tert-butyl 4-(benzylamino)-3,3-difluoropiperidine-1-carboxylate. LC-MS-conditions 08: tR=0.65 min; [M+H]+=327.32.

後処理

  1. extractionextracted with EA (3×50 mL)
  2. dry with materialThe combined organic extracts were dried over MgSO4
  3. filtrationfiltered
  4. customthe solvent removed under reduced pressure
  5. customThe residue was purified by FC (Heptane/EA, 1:1)

出典と根拠

ORDレコード
ord-4499ac85e7464dd28838beef3fef46b6
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09139524B2

反応ノート

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