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

HRID 1044782노트

반응식

HRID 1044782 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

반응 조건

온도
0 °C

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 (1.84 g, 9.59 mmol) in MeOH (20 mL) was added NaBH4 (456 mg, 12.05 mmol in four portions). The reaction mixture was then stirred for 1 h at 0° C. 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 pale yellow oil. TLC:rf (4:1 hept-EA)=0.12. LC-MS-conditions 02: tR=0.74 min.

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-33f59c34cd6941688d5d17628315b61b
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08563714B2

반응 노트

불러오는 중…