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

Triphenylphosphine → 3-[4-(2-Pyridinylamino)butoxy]phenyl-3-methylbutanoic acid

HRID 2085057
노트
인쇄 미리보기

반응식

HRID 2085057 반응식
N1C=CC=CC=1N[CH2:8][CH2:9][CH2:10][O:11][C:12]1[CH:13]=[C:14]([CH:18]([CH:22]([CH3:24])[CH3:23])[C:19]([OH:21])=[O:20])[CH:15]=[CH:16][CH:17]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.OCCC[CH2:48][NH:49][C:50]1[CH:55]=[CH:54][CH:53]=[CH:52][N+:51]=1[O-].N(C(OCC)=O)=NC(OCC)=O>CN(C=O)C>[N:51]1[CH:52]=[CH:53][CH:54]=[CH:55][C:50]=1[NH:49][CH2:48][CH2:8][CH2:9][CH2:10][O:11][C:12]1[CH:13]=[C:14]([CH:18]([CH:22]([CH3:23])[CH3:24])[C:19]([OH:21])=[O:20])[CH:15]=[CH:16][CH:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 226027013-[3-(2-Pyridinylamino)propoxy]phenyl-3-methylbutanoic acidHCID 178526250HCID 178526250, 화합물

생성물 1

HCID 226026993-[4-(2-Pyridinylamino)butoxy]phenyl-3-methylbutanoic acid수율 50.5%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매
2회

실험 절차

To a solution of the product from Example 5, Step 3 (720 mg, 3.24 mmol) in DMF (9 mL) was added triphenylphosphine (850 mg, 3.24 mmol). The reaction solution was kept at ambient temperature for 1 hour and a solution of 2-(4-hydroxybutylamino)pyridine N-oxide (590 mg, 3.24 mmol) and diethyl azodicarboxylate (0.51 mL, 3.24 mmol) in DMF (5 mL) was added. The reaction solution was kept at room temperature for 18 hours and concentrated in vacuo. The residue was dissolved in ethyl acetate and washed with water. The aqueous solution was back extracted with ethyl acetate. The combined organic solution was washed with brine, dried (Na2SO4) and concentrated in vacuo. The residue was purified by chromatography (98:1:1 CH2Cl2:MeOH:NH4OH) to give the desired product, (560 mg, 45% yield).

후처리

  1. waitThe reaction solution was kept at room temperature for 18 hours
  2. concentrationconcentrated in vacuo
  3. dissolutionThe residue was dissolved in ethyl acetate
  4. washwashed with water
  5. extractionThe aqueous solution was back extracted with ethyl acetate
  6. washThe combined organic solution was washed with brine
  7. dry with materialdried (Na2SO4)
  8. concentrationconcentrated in vacuo
  9. customThe residue was purified by chromatography (98:1:1 CH2Cl2:MeOH:NH4OH)

출처 및 근거

ORD 기록
ord-079ac4cdb2aa49b08a17a38bc4e72864
출처 데이터셋
uspto-grants-2004_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06720315B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트