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Methylamine → 1-(1,3-Benzoxazol-2-yl)-N-methylmethanamine

HRID 1030265
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HRID 1030265 반응식
Cl[CH2:2][C:3]1[O:4][C:5]2[CH:11]=[CH:10][CH:9]=[CH:8][C:6]=2[N:7]=1.[CH3:12][NH2:13]>O>[CH3:12][NH:13][CH2:2][C:3]1[O:4][C:5]2[CH:11]=[CH:10][CH:9]=[CH:8][C:6]=2[N:7]=1
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참가 물질

4

반응물 2

HCID 6329MethylamineHCID 20619892-(Chloromethyl)-1,3-benzoxazole

생성물 1

HCID 156759021-(1,3-Benzoxazol-2-yl)-N-methylmethanamine수율 82%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

2-(Chloromethyl)benzoxazole (3.99 g, 23.8 mmol) was dissolved in aqueous methylamine (40 mL, 40 wt % in H2O) at 10° C. under a nitrogen atmosphere. After 20 minutes, the reaction mixture was warmed to room temperature and stirred for 1 hour. The mixture was diluted with water and extracted with methylene chloride. The organic phase was dried (MgSO4) and concentrated to afford crude product which was purified by flash column chromatography (5% MeOH/CH2Cl2) to afford 3.18 g (82%) of pure product as a yellow oil.

후처리

  1. extractionextracted with methylene chloride
  2. dry with materialThe organic phase was dried (MgSO4)
  3. concentrationconcentrated
  4. customto afford crude product which
  5. customwas purified by flash column chromatography (5% MeOH/CH2Cl2)

출처 및 근거

ORD 기록
ord-4d3a1ef2010e40fba525942b0186312d
출처 데이터셋
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05104892

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