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

HRID 26731
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HRID 26731 반응식
[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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
50 °C

실험 절차

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 1N 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; m.p. 131°-133° C.; beige, amorphous powder.

후처리

  1. additionAfter the addition
  2. customThe solvent is evaporated
  3. dissolutionThe oily residue is dissolved in 150 parts of hydrochloric acid 1N
  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

출처 및 근거

ORD 기록
ord-b6aa8350907c43e2a1b31831c8e011fc
출처 데이터셋
uspto-grants-1979_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04151286

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