Sodium Bicarbonate → HCID 59177295, 화합물

HRID 2076801노트

반응식

HRID 2076801 반응식
[C:1]1([C@@H:7]2[O:12][CH2:11][CH2:10][NH:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl:13][C:14]1[N:19]=[CH:18][C:17]([CH:20]=O)=[CH:16][CH:15]=1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)(O)[O-].[Na+]>ClC(Cl)C>[Cl:13][C:14]1[N:19]=[CH:18][C:17]([CH2:20][N:9]2[CH2:10][CH2:11][O:12][C@@H:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[CH2:8]2)=[CH:16][CH:15]=1

참가 물질

6

반응물 4

HCID 516892Sodium BicarbonateHCID 937783(2S)-2-PhenylmorpholineHCID 27640536-Chloropyridine-3-carbaldehydeHCID 5049666Sodium triacetoxyborohydride

생성물 1

HCID 59177295HCID 59177295, 화합물수율 63.5%

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

실험 절차

10 g of (S)-2-Phenyl-morpholine was dissolved in 610 mL of dichloroethane. 10.407 g of 6-Chloropyridine-3-carboxaldehyde was added and the reaction stirred at room temperature for 30 minutes followed by addition of 23.4 g of sodium triacetoxyborohydride. After stirring overnight at room temperature, the solution was poured into an aqueous saturated sodium bicarbonate solution and the layers separated. The organic layer was washed several times with aqueous saturated sodium bicarbonate solution followed by brine. It was then dried over sodium sulfate, filtered and concentrated in vacuo. Purification was accomplished by flash chromatography to afford 11.23 g of product. 63.5% yield. EI m/z 289=MH+

후처리

  1. stirringAfter stirring overnight at room temperature
  2. customthe layers separated
  3. washThe organic layer was washed several times with aqueous saturated sodium bicarbonate solution
  4. dry with materialIt was then dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customPurification

출처 및 근거

ORD 기록
ord-42d9c266a6524a7caaa7d7da320ac266
출처 데이터셋
uspto-grants-2011_04
특허 번호
US07928103B2

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