Benzyl Bromide → HCID 16459886、化合物

HRID 1457610ノート

反応式

HRID 1457610 の反応式
[NH:1]1[CH2:6][CH2:5][CH:4]([CH2:7][NH:8][CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH2:3][CH2:2]1.[CH2:16](Br)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>O1CCCC1>[CH2:16]([N:1]1[CH2:2][CH2:3][CH:4]([CH2:7][NH:8][CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH2:5][CH2:6]1)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1

参加物

4

反応物 2

HCID 7498Benzyl BromideHCID 16004294N-(Phenylmethyl)-4-piperidinemethanamine

生成物 1

HCID 16459886HCID 16459886、化合物収率 50%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Under ice-cooling, to 200 ml of a tetrahydrofuran (THF) solution containing 5.0 g of N-(4-piperidylmethyl)-N-benzylamine was added dropwise 50 ml of a THF solution containing 2.9 ml of benzyl bromide. After stirring the mixture at the same temperature for one hour, THF was removed from the reaction mixture under reduced pressure and a saturated sodium hydrogen carbonate aqueous solution was added to the residue. The mixture was extracted with ethyl acetate. The extract was washed and dried, and the solvent was removed under reduced pressure. Precipitated crystals were recrystallized from an ethanol solution to give 3.6 g of N-(1-benzylpiperidin-4-ylmethyl)-N-benzylamine (yield: 50%, melting point: 240° C. or higher).

後処理

  1. customTHF was removed from the reaction mixture under reduced pressure
  2. additiona saturated sodium hydrogen carbonate aqueous solution was added to the residue
  3. extractionThe mixture was extracted with ethyl acetate
  4. washThe extract was washed
  5. customdried
  6. customthe solvent was removed under reduced pressure
  7. customPrecipitated crystals
  8. customwere recrystallized from an ethanol solution

出典と根拠

ORDレコード
ord-becb89b4c28341b3b0e97a7d16d6830a
出典データセット
uspto-grants-1998_12
特許番号
US05849732

反応ノート

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