Sodium Hydroxide → (Azepan-4-yl)methanol

HRID 1620560노트

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HRID 1620560 반응식
O=[C:2]1[NH:8][CH2:7][CH2:6][CH:5]([C:9]([O-])=[O:10])[CH2:4][CH2:3]1.[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[Na+]>C1COCC1.O>[NH:8]1[CH2:2][CH2:3][CH2:4][CH:5]([CH2:9][OH:10])[CH2:6][CH2:7]1

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 866787397-Oxoazepane-4-carboxylate

생성물 1

HCID 22594076(Azepan-4-yl)methanol수율 84.4%

시약·촉매·용매 2

HCID 962Water용매2회HCID 8028Tetrahydrofuran용매3회

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온도
60 °C

실험 절차

A solution of the obtained 7-oxoazepane-4-carboxylate (2.02 g) in THF (29 mL) was added dropwise to a suspension of lithium aluminum hydride (2.07 g) in THF (80 mL) under ice-cooling. The reaction mixture was stirred at room temperature for 3 hr and at 60° C. overnight. The reaction mixture was ice-cooled, diluted with THF (200 mL), and water (2.02 mL) was slowly added dropwise. Furthermore, 15% aqueous sodium hydroxide solution (2.02 mL) was added dropwise, then water (4.04 mL) was added, and the mixture was stirred at room temperature for 3 hr. The solid was separated by filtration, and the filtrate was concentrated under reduced pressure to give the title compound (1.41 g).

후처리

  1. temperaturecooling
  2. temperaturecooled
  3. additionwas slowly added dropwise
  4. stirringthe mixture was stirred at room temperature for 3 hr
  5. customThe solid was separated by filtration
  6. concentrationthe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-956f31ec38a747649b20433590197912
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08772277B2

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