홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Triethylamine → HCID 12985692, 화합물

HRID 2184221
노트
인쇄 미리보기

반응식

HRID 2184221 반응식
[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][C:15]([N:17]2[CH2:22][CH2:21][CH:20]([OH:23])[CH2:19][CH2:18]2)=[O:16])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.[S:31](Cl)([CH3:34])(=[O:33])=[O:32]>C1(C)C=CC=CC=1>[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][C:15]([N:17]2[CH2:22][CH2:21][CH:20]([O:23][S:31]([CH3:34])(=[O:33])=[O:32])[CH2:19][CH2:18]2)=[O:16])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 10381067HCID 10381067, 화합물

생성물 1

HCID 12985692HCID 12985692, 화합물수율 84.7%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
66 °C

실험 절차

To a mixture of 4.75 g (0.015 mol) of 1-(1-benzyl-4-piperidylacetyl)-4-hydroxypiperidine [1], 51 g of toluene, 1.68 g (0.017 mol) of triethylamine, 1.87 g (0.016 mol) of mesyl chloride was added dropwise at a temperature in the range of 0 to 10° C. and the reaction was allowed to proceed for 2 hours at the temperature in the range. Thereafter, the reaction mixture was washed with an aqueous solution of sodium hydrogencarbonate and an aqueous solution of sodium chloride. The resultant organic layer was dried with anhydrous magnesium sulfate and concentrated under a reduced pressure. To the concentrated residue, 7 g of 2-propanol and 43 g of diisopropyl ether were added and the temperature of the mixture was increased. The mixture was stirred for 0.3 hours at a reflux temperature of 66° C. Thereafter the mixture was cooled to room temperature and subjected to filtration. The resultant wet crystal was dried under a reduced pressure, whereby 5.01 g of the title compound in the state of white powder was obtained (the yield was 84.7%).

후처리

  1. additionwas added dropwise at a temperature in the range of 0 to 10° C.
  2. washThereafter, the reaction mixture was washed with an aqueous solution of sodium hydrogencarbonate
  3. dry with materialThe resultant organic layer was dried with anhydrous magnesium sulfate
  4. concentrationconcentrated under a reduced pressure
  5. additionTo the concentrated residue, 7 g of 2-propanol and 43 g of diisopropyl ether were added
  6. temperaturethe temperature of the mixture was increased
  7. temperatureThereafter the mixture was cooled to room temperature
  8. filtrationsubjected to filtration
  9. dry with materialThe resultant wet crystal was dried under a reduced pressure, whereby 5.01 g of the title compound in the state of white powder
  10. customwas obtained (the yield was 84.7%)

출처 및 근거

ORD 기록
ord-74165972a08c4f319d9c55a453758981
출처 데이터셋
uspto-grants-2005_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06900326B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트