2-Methyl-2-butanol → HCID 178526251, 화합물

HRID 497547

반응식

HRID 497547 반응식
Cl[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][N+:3]=1[O-:8].[NH2:9][CH2:10][CH2:11][CH2:12][OH:13].C([O-])(O)=O.[Na+].C(O)(CC)(C)C>C(Cl)Cl>[OH:13][CH2:12][CH2:11][CH2:10][NH:9][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][N+:3]=1[O-:8]

참가 물질

6

반응물 4

HCID 64052-Methyl-2-butanolHCID 90863-Amino-1-propanolHCID 754652-Chloropyridine oxideHCID 516892Sodium Bicarbonate

생성물 1

HCID 178526251HCID 178526251, 화합물수율 80.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
67 °C

실험 절차

A mixture of 2-chloropyridine-N-oxide (16.6 g, 100 mmoles), 3-amino-1-propanol (15.3 ml, 200 mmoles), NaHCO3 (42 g, 0.5 mole), and tert-amyl alcohol (100 ml) was heated to reflux. After 23 hours, the reaction was cooled, diluted with CH2Cl2 (300 ml), and filtered to remove insoluble materials. The filtrate was concentrated to afford a brown oil. The oil was dried under vacuum overnight. Ether (100 ml) was added to give a brown solid. The ether was decanted and the solid was washed further with ether/acetonitrile (3/1). The resulting solid was heated at 67° C. under vacuum to give the desired product (13.5 g). 1H NMR was consistent with the proposed structure.

후처리

  1. temperaturewas heated to reflux
  2. temperaturethe reaction was cooled
  3. filtrationfiltered
  4. customto remove insoluble materials
  5. concentrationThe filtrate was concentrated
  6. customto afford a brown oil
  7. customThe oil was dried under vacuum overnight
  8. additionEther (100 ml) was added
  9. customto give a brown solid
  10. customThe ether was decanted
  11. washthe solid was washed further with ether/acetonitrile (3/1)

출처 및 근거

ORD 기록
ord-7638cfb683b8452eb81dd8e69519514f
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06949578B2

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