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

Diisopropylamine → HCID 9907318, 화합물

HRID 49958
노트
인쇄 미리보기

반응식

HRID 49958 반응식
[CH3:1][O:2][C:3]1[CH:13]=[CH:12][C:6]([N:7]([CH3:11])[C:8](=[O:10])[CH3:9])=[CH:5][CH:4]=1.C([N-]C(C)C)(C)C.[Li+].C(NC(C)C)(C)C.C([Li])CCC.[CH2:34]([N:41]1[CH2:46][CH2:45][C:44](=[O:47])[CH2:43][CH2:42]1)[C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1>O.O1CCCC1>[CH3:1][O:2][C:3]1[CH:13]=[CH:12][C:6]([N:7]([CH3:11])[C:8](=[O:10])[CH2:9][C:44]2([OH:47])[CH2:45][CH2:46][N:41]([CH2:34][C:35]3[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=3)[CH2:42][CH2:43]2)=[CH:5][CH:4]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 7912DiisopropylamineHCID 192201-Benzyl-4-piperidoneHCID 142032Acetamide, N-(4-methoxyphenyl)-N-methyl-HCID 2724682Lithium diisopropylamideHCID 178418339Butyllithium

생성물 1

HCID 9907318HCID 9907318, 화합물수율 69.7%

시약·촉매·용매 2

HCID 962Water용매
HCID 8028Tetrahydrofuran용매3회

반응 조건

온도
-78 °C

실험 절차

A solution of 4′-methoxy-N-methylacetanilide (12 g) in an anhydrous tetrahydrofuran (30 mL) was added to a solution in an anhydrous tetrahydrofuran (100 mL) of lithium diisopropylamide prepared from diisopropylamine (10.5 mL) and n-butyl lithium (1.53M hexane solution; 48 mL) at below −65° C., and the mixture was stirred at −78° C. for 15 minutes. An anhydrous tetrahydrofuran solution (20 mL) of 1-benzylpiperidin-4-one (12.7 g) was then added to this reaction mixture at below −65° C., and the resulting mixture was stirred at −78° C. for 10 minutes. After increasing the temperature to room temperature, water was added to the mixture, and the mixed solution was extracted with ethyl acetate. The organic layer was washed with water and saturated brine and dried over anhydrous sodium sulfate, followed by distilling off the solvent under reduced pressure. The residue obtained was recrystallized from ether-hexane to obtain the titled compound (17.2 g).

후처리

  1. stirringthe resulting mixture was stirred at −78° C. for 10 minutes
  2. temperatureAfter increasing the temperature to room temperature
  3. extractionthe mixed solution was extracted with ethyl acetate
  4. washThe organic layer was washed with water and saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationby distilling off the solvent under reduced pressure
  7. customThe residue obtained
  8. customwas recrystallized from ether-hexane

출처 및 근거

ORD 기록
ord-7da2c7e3439d4fd09da343e794317901
출처 데이터셋
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06710060B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트