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

Triphenylphosphine → HCID 58381698, 화합물

HRID 410044
노트
인쇄 미리보기

반응식

HRID 410044 반응식
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.CC(OC(/N=N/C(OC(C)C)=O)=O)C.[CH2:34](O)[CH2:35][CH2:36][CH2:37]/[CH:38]=[CH:39]\[CH2:40]/[CH:41]=[CH:42]\[CH2:43]/[CH:44]=[CH:45]\[CH2:46]/[CH:47]=[CH:48]\[CH2:49]/[CH:50]=[CH:51]\[CH2:52][CH3:53].[C:55]([OH:58])(=[S:57])[CH3:56]>C1COCC1.CCCCCCC>[C:55](=[O:58])([S:57][CH2:34][CH2:35][CH2:36][CH2:37]/[CH:38]=[CH:39]\[CH2:40]/[CH:41]=[CH:42]\[CH2:43]/[CH:44]=[CH:45]\[CH2:46]/[CH:47]=[CH:48]\[CH2:49]/[CH:50]=[CH:51]\[CH2:52][CH3:53])[CH3:56]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 11776TriphenylphosphineHCID 5363146Diisopropyl azodicarboxylateHCID 59539494(5Z,8Z,11Z,14Z,17Z)-icosa-5,8,11,14,17-pentaen-1-olHCID 178418634HCID 178418634, 화합물

생성물 1

HCID 58381698HCID 58381698, 화합물수율 79.3%

시약·촉매·용매 2

HCID 8028
Tetrahydrofuran
용매
2회
HCID 8900Heptane용매

반응 조건

온도
0 °C

실험 절차

Triphenylphosphine (21.0 g, 80 mmol) was dissolved in dry THF (170 mL) at 0° C. under inert atmosphere and added DIAD (15.8 mL, 80 mmol) dropwise. After 40 minutes at 0° C. the white suspension was added dropwise to a solution of (5Z,8Z,11Z,14Z,17Z)-icosa-5,8,11,14,17-pentaen-1-ol (11.5 g, 40 mmol) and thioacetic acid (5.7 mL, 80 mmol) in dry THF (50 mL) during 15 minutes. The resulting turbid mixture was stirred at 0° C. for 30 minutes, followed by ambient temperature for 1.5 hour. Heptane was added (200 mL), the mixture was stirred for ten minutes and the precipitated white solid removed by filtration and rinsed with heptane (150 mL). The residue was concentrated to remove most of the THF and stirred at ambient for 18 hours. The mixture was filtered, concentrated and added heptane (200 mL). The resulting mixture was stirred for 2 hours, filtered and evaporated. The residue was purified by flash chromatography on silica gel, using EtOAc:Heptane (2:98), followed by EtOAc:Heptane (4:96) and finally EtOAc:Heptane (5:95). Concentration of the appropriate fractions provided 11.0 g (79% yield) of the title compound as oil.

후처리

  1. waitfollowed by ambient temperature for 1.5 hour
  2. stirringthe mixture was stirred for ten minutes
  3. customthe precipitated white solid removed by filtration
  4. washrinsed with heptane (150 mL)
  5. concentrationThe residue was concentrated
  6. customto remove most of the THF
  7. stirringstirred at ambient for 18 hours
  8. filtrationThe mixture was filtered
  9. concentrationconcentrated
  10. additionadded heptane (200 mL)
  11. stirringThe resulting mixture was stirred for 2 hours
  12. filtrationfiltered
  13. customevaporated
  14. customThe residue was purified by flash chromatography on silica gel

출처 및 근거

ORD 기록
ord-2c7c0fa7108f491db856cdf084b8b11f
출처 데이터셋
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08759558B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트