Sodium borohydride → 2,2-diethoxy-N-(thiophen-2-ylmethyl)ethanamine

HRID 1511595노트

반응식

HRID 1511595 반응식
[CH2:1]([O:3][CH:4]([O:13][CH2:14][CH3:15])[CH2:5][N:6]=[CH:7][C:8]1[S:9][CH:10]=[CH:11][CH:12]=1)[CH3:2].[BH4-].[Na+]>C(O)C>[CH2:14]([O:13][CH:4]([O:3][CH2:1][CH3:2])[CH2:5][NH:6][CH2:7][C:8]1[S:9][CH:10]=[CH:11][CH:12]=1)[CH3:15]

참가 물질

4

반응물 2

HCID 4311764Sodium borohydrideHCID 218211702,2-Diethoxy-N-(thiophen-2-ylmethylene)ethaneamine

생성물 1

HCID 27953962,2-diethoxy-N-(thiophen-2-ylmethyl)ethanamine수율 71.9%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

2,2-Diethoxy-N-(thiophen-2-ylmethylene)ethaneamine (100 g) prepared in the step 1 was dissolved in 500 mL of dry ethanol, then 18.3 g of sodium borohydride was slowly added thereto little by little at room temperature and the mixture was stirred overnight at room temperature. The solvent was evaporated from the reaction solution in vacuo and the residue was poured over 300 mL of a 10% aqueous solution of acetic acid. The resulting aqueous solution was washed with diethyl ether, neutralized with 10% aqueous ammonia and subjected to extraction with diethyl ether. The organic layer was washed with water and a saturated solution of sodium chloride successively and dried over anhydrous magnesium sulfate and the solvent was evaporated therefrom in vacuo to give 72.5 g of the objective compound as colorless liquid.

후처리

  1. customThe solvent was evaporated from the reaction solution in vacuo
  2. additionthe residue was poured over 300 mL of a 10% aqueous solution of acetic acid
  3. washThe resulting aqueous solution was washed with diethyl ether
  4. extractionsubjected to extraction with diethyl ether
  5. washThe organic layer was washed with water
  6. dry with materiala saturated solution of sodium chloride successively and dried over anhydrous magnesium sulfate
  7. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-d5921d32063e4ba0b245f82bc0d86b5c
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08217031B2

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