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Monobenzone → (S)-1-(4-benzyloxyphenoxy)-3-[N-mesyl-(1-methylethyl)amino]-2-propanol

HRID 2417975
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HRID 2417975 반응식
[CH3:1][CH:2]([N:4]([S:9]([CH3:12])(=[O:11])=[O:10])[CH2:5][C@H:6]1[CH2:8][O:7]1)[CH3:3].[CH2:13]([O:20][C:21]1[CH:26]=[CH:25][C:24]([OH:27])=[CH:23][CH:22]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.CC(C)([O-])C.[K+]>CO.[OH-].[Na+]>[CH2:13]([O:20][C:21]1[CH:22]=[CH:23][C:24]([O:27][CH2:8][C@@H:6]([OH:7])[CH2:5][N:4]([CH:2]([CH3:3])[CH3:1])[S:9]([CH3:12])(=[O:11])=[O:10])=[CH:25][CH:26]=1)[C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 7638MonobenzoneHCID 13208807(S)-N-(1-methylethyl)-N-(methylsulfonyl)oxiranemethaneamineHCID 23665647Potassium tert-butoxide

생성물 1

HCID 12952555(S)-1-(4-benzyloxyphenoxy)-3-[N-mesyl-(1-methylethyl)amino]-2-propanol수율 88.7%

시약·촉매·용매 2

HCID 887Methanol용매
HCID 14798
Sodium Hydroxide
용매
2회

실험 절차

To a solution of (S)-N-(1-methylethyl)-N-(methylsulfonyl)oxiranemethaneamine (86.98 g) and 4-benzyloxyphenol (100 g) in 100 ml methanol was added potassium t-butoxide (5.04 g) and the mixture was stirred under reflux for 16 hours, whereupon 150 ml 2N sodium hydroxide was added and the reaction turned to a solid mass. It was diluted further with 1 L 1N sodium hydroxide solution and stirred for 1 hour to digest the solids which were then removed by filtration, washed with 1N sodium hydroxide and with water. The still wet crude material was taken up in dichloromethane, and the solution was dried over sodium sulfate and partially evaporated in vacuo to a thick oil (wt 250 g) which was then diluted with stirring using 1 L of ether. The mixture was chilled and the product filtered to give 157.1 g of (S)-1-(4-benzyloxyphenoxy)-3-[N-mesyl-(1-methylethyl)amino]-2-propanol, mp 96°-97°.

후처리

  1. additionwas added
  2. stirringstirred for 1 hour
  3. customwere then removed by filtration
  4. washwashed with 1N sodium hydroxide and with water
  5. dry with materialthe solution was dried over sodium sulfate
  6. custompartially evaporated in vacuo to a thick oil (wt 250 g) which
  7. additionwas then diluted
  8. stirringwith stirring
  9. temperatureThe mixture was chilled
  10. filtrationthe product filtered

출처 및 근거

ORD 기록
ord-540cb2d1be0643bcb44f93976965c36d
출처 데이터셋
uspto-grants-1984_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04471116

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