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Sodium borohydride → N-[1-(phenylmethyl)-4-piperidinyl]-3-pyridinamine

HRID 236734
ノート
印刷プレビュー

反応式

HRID 236734 の反応式
[C:1]1([CH2:7][N:8]2[CH2:13][CH2:12][C:11](=[N:14][C:15]3[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=3)[CH2:10][CH2:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[BH4-].[Na+]>C(O)C>[C:1]1([CH2:7][N:8]2[CH2:9][CH2:10][CH:11]([NH:14][C:15]3[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=3)[CH2:12][CH2:13]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=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

4

反応物 2

HCID 4311764Sodium borohydrideHCID 10706822N-[1-(phenylmethyl)-4-piperidinylidene]-3-pyridinamine

生成物 1

HCID 10706957N-[1-(phenylmethyl)-4-piperidinyl]-3-pyridinamine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
50 °C

実験手順

To a stirred solution of 27 parts of N-[1-(phenylmethyl)-4-piperidinylidene]-3-pyridinamine in 40 parts of ethanol are added portionwise 3.8 parts of sodium borohydride. After the addition is complete, the whole is heated to 50° C. The solvent is evaporated. The oily residue is dissolved in 150 parts of hydrochloric acid 1 N and filtered. The filtrate is rendered alkaline with ammonium hydroxide and extracted with methylbenzene. The organic layer is dried over magnesium sulfate, filtered and evaporated. The solid residue is washed with 2,2'-oxybispropane and dried, yielding 14 parts of N-[1-(phenylmethyl)-4-piperidinyl]-3-pyridinamine; mp. 131°-133° C.; beige, amorphous powder.

後処理

  1. additionAfter the addition
  2. customThe solvent is evaporated
  3. dissolutionThe oily residue is dissolved in 150 parts of hydrochloric acid 1 N
  4. filtrationfiltered
  5. extractionextracted with methylbenzene
  6. dry with materialThe organic layer is dried over magnesium sulfate
  7. filtrationfiltered
  8. customevaporated
  9. washThe solid residue is washed with 2,2'-oxybispropane
  10. customdried

出典と根拠

ORDレコード
ord-d3bafbd3a7c1427bb4ec3c1c4d13b7bb
出典データセット
uspto-grants-1979_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04157393

反応ノート

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