Nitrogen → [3-(2-Methyl-[1,3]dioxolan-2-yl)-phenyl]-methanol

HRID 2064980노트

반응식

HRID 2064980 반응식
N#N.[CH3:3][C:4]1([C:9]2[CH:10]=[C:11]([CH:14]=[CH:15][CH:16]=2)[CH:12]=[O:13])[O:8][CH2:7][CH2:6][O:5]1.[BH4-].[Na+].O>CO>[CH3:3][C:4]1([C:9]2[CH:10]=[C:11]([CH2:12][OH:13])[CH:14]=[CH:15][CH:16]=2)[O:5][CH2:6][CH2:7][O:8]1

참가 물질

6

반응물 4

HCID 947NitrogenHCID 962WaterHCID 4311764Sodium borohydrideHCID 10607757Benzaldehyde, 3-(2-methyl-1,3-dioxolan-2-yl)-

생성물 1

HCID 66820167[3-(2-Methyl-[1,3]dioxolan-2-yl)-phenyl]-methanol

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), to a ice-cold solution of 3-(2-methyl-[1,3]dioxolan-2-yl)-benzaldehyde (896 mg, 4.66 mmol) in MeOH (10.0 mL) was added NaBH4 (228 mg, 5.79 mmol in four equal portions). The reaction mixture was then stirred at rt for 1 h. Water was added and the mixture was extracted twice with EA. The combined org. extracts were washed with brine, dried over Na2SO4, filtered, and the solvent was removed under reduced pressure to give the title compound as a colorless oil. TLC: rf (50:50 hept-EA)=0.28. LC-MS-conditions 02: tR=0.74 min; [M+H]+=195.71.

후처리

  1. extractionthe mixture was extracted twice with EA
  2. washextracts were washed with brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. customthe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-56bd233b3a234fe794f280f190f9f744
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08288419B2

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