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Benzylamine → N-benzyl [(2S)-1-benzylpiperidin-2-ylmethyl]amine

HRID 1006330
ノート
印刷プレビュー

反応式

HRID 1006330 の反応式
C(Cl)(=O)C(Cl)=O.C(=O)=O.CC(C)=O.[CH2:14]([N:21]1[CH2:26][CH2:25][CH2:24][CH2:23][C@H:22]1[CH2:27]O)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.[CH2:29]([NH2:36])[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)([O-])O.[Na+]>ClCCl.ClCCCl.O.C(N(CC)CC)C.CS(C)=O>[CH2:29]([NH:36][CH2:27][C@@H:22]1[CH2:23][CH2:24][CH2:25][CH2:26][N:21]1[CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

12

反応物 6

HCID 7504BenzylamineHCID 65578Oxalyl chlorideHCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 7021240(S)-(1-benzylpiperidin-2-yl)methanolHCID 18522661Acetone cardice

生成物 1

HCID 69819710
N-benzyl [(2S)-1-benzylpiperidin-2-ylmethyl]amine

試薬・触媒・溶媒 5

HCID 111,2-Dichloroethane溶媒HCID 679Dimethyl Sulfoxide溶媒HCID 962Water溶媒HCID 6344Dichloromethane溶媒3 回HCID 8471Triethylamine溶媒

実験手順

A solution of dimethyl sulfoxide (0.219 ml) in dichloromethane (1.1 ml) was added dropwise to a solution of oxalyl chloride (0.133 ml) in dichloromethane (2.7 ml) under cooling below −60° C. with dry ice-acetone. After 5 minutes, the mixture was allowed to −10° C., and a solution of (2S)-1-benzyl-2-(hydroxymethyl)piperidine (156.5 mg) in dichloromethane (1.6 ml) was added to the mixture. The whole mixture was then cooled below −60° C. and was stirred for 20 minutes at the same temperature. After addition of triethylamine (0.64 ml) followed by stirring at room temperature, the reaction mixture was poured into water and extracted with 1,2-dichloroethane. The extract was dried over magnesium sulfate and evaporated under reduced pressure to give a syrup. Benzylamine (0.33 ml) was added to the solution of the syrup obtained above procedure in 1,2-dichloroethane (2.5 ml) with ice-cooling. After the whole was stirred for 30 minutes at the same temperature, sodium triacetoxyborohydride (0.323 g) was added to this mixture. The reaction mixture was allowed to room temperature and was stirred for 3 hours. The mixture was poured into aqueous saturated sodium hydrogen carbonate solution and extracted with dichloromethane. The extract was dried over magnesium sulfate and evaporated under reduced pressure. The resulting residue was purified by silica gel chromatography using a mixture of dichloromethane and methanol (20:1) as an eluent to give N-benzyl-[(2S)-1-benzylpiperidin-2-ylmethyl]amine (168.5 mg).

後処理

  1. customwas allowed to −10° C.
  2. temperatureThe whole mixture was then cooled below −60° C.
  3. stirringby stirring at room temperature
  4. extractionextracted with 1,2-dichloroethane
  5. dry with materialThe extract was dried over magnesium sulfate
  6. customevaporated under reduced pressure
  7. customto give a syrup
  8. temperaturecooling
  9. additionwas added to this mixture
  10. customwas allowed to room temperature
  11. stirringwas stirred for 3 hours
  12. extractionextracted with dichloromethane
  13. dry with materialThe extract was dried over magnesium sulfate
  14. customevaporated under reduced pressure
  15. customThe resulting residue was purified by silica gel chromatography
  16. additiona mixture of dichloromethane and methanol (20:1) as an eluent

出典と根拠

ORDレコード
ord-ac28a86fe3484b7c86b5e61478ff6834
出典データセット
uspto-grants-2004_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06787543B2

反応ノート

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