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

Triphenylphosphine → HCID 68408307, 화합물

HRID 1176163
노트
인쇄 미리보기

반응식

HRID 1176163 반응식
[CH2:1]([O:13][C:14]1[CH:19]=[CH:18][C:17](I)=[CH:16][CH:15]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[CH3:40][Si:41]([C:44]#[CH:45])([CH3:43])[CH3:42].[NH4+].[Cl-]>N1CCCCC1.[Cu]I.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[CH2:1]([O:13][C:14]1[CH:19]=[CH:18][C:17]([C:45]#[C:44][Si:41]([CH3:43])([CH3:42])[CH3:40])=[CH:16][CH:15]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 11776TriphenylphosphineHCID 25517Ammonium ChlorideHCID 66111TrimethylsilylacetyleneHCID 10883601Benzene, 1-(dodecyloxy)-4-iodo-

생성물 1

HCID 68408307HCID 68408307, 화합물

시약·촉매·용매 3

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
촉매
HCID 178418476HCID 178418476, 화합물촉매
HCID 8082Piperidine용매

반응 조건

온도
50 °C

실험 절차

4-(Dodecyloxy)iodobenzene (4.04 g, 1.04×10−2 mol), triphenylphosphine (0.165 g, 6.29×10−4 mol), CuI (0.108 g, 5.67×10−4 mol) and Pd(PPh3)2Cl2 (0.153 g, 2.18×10−4 mol) were dissolved in 40 ml of dry piperidine under N2. (Trimethylsilyl)acetylene (3.00 ml, 2.12×10−2 mol) was added and the mixture was stirred at 50° C. for 6 h under N2. After cooling, the reaction mixture was poured into aq. NH4Cl and extracted with CH2Cl2 (three times). The combined organic layers were washed with aq. NH4Cl, water, and dried over Na2SO4. The crude product was chromatographed on silica gel with 4:1 hexane:CH2Cl2 as the eluent. Yield=3.633 g (97% based on 4.04 g of 4-(dodecyloxy)iodobenzene). 1H NMR (250 MHz, CDCl3): δ 7.39 (d, 2H, J=8.9 Hz, Ph), 6.80 (d, 2H, J=9.0 Hz, Ph), 3.94 (t, 2H, J=6.6 Hz, —OCH2—), 1.77 (quint, 2H, J=6.6 Hz, —OCH2CH2—), 1.17-1.50 (m, 18H, —CH2—), 0.88 (t, 3H, J=6.6 Hz, —CH3), 0.24 (s, 9H, Si—CH3). CI MS m/z: 358.268 (M+) (calcd 358.269).

후처리

  1. temperatureAfter cooling
  2. extractionextracted with CH2Cl2 (three times)
  3. washThe combined organic layers were washed with aq. NH4Cl, water
  4. dry with materialdried over Na2SO4
  5. customThe crude product was chromatographed on silica gel with 4:1 hexane

출처 및 근거

ORD 기록
ord-06155a86bd304016abeaf05e10819f05
출처 데이터셋
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07842758B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트