Diphenyl Ether → Di-n-octylphosphinic acid

HRID 625204

반응식

HRID 625204 반응식
C1([O:7]C2C=CC=CC=2)C=CC=CC=1.C(O)(=O)CCCCCCC/C=C\CCCCCCCC.C(N)CCCCCCC/C=C\CCCCCCCC.[Se].C(P(CCCCCCCC)CCCCCCCC)CCCCCCC.C([P:87](=[O:104])([CH2:96][CH2:97][CH2:98][CH2:99][CH2:100][CH2:101][CH2:102][CH3:103])[CH2:88][CH2:89][CH2:90][CH2:91][CH2:92][CH2:93][CH2:94][CH3:95])CCCCCCC>C=CCCCCCCCCCCCCCCCC.CN1C(=O)CCC1.C1(C)C=CC=CC=1.CO.C(#N)C>[CH2:96]([P:87]([CH2:88][CH2:89][CH2:90][CH2:91][CH2:92][CH2:93][CH2:94][CH3:95])(=[O:104])[OH:7])[CH2:97][CH2:98][CH2:99][CH2:100][CH2:101][CH2:102][CH3:103]

참가 물질

12

반응물 6

HCID 7583Diphenyl EtherHCID 20851TrioctylphosphineHCID 65577Trioctylphosphine oxideHCID 445639Oleic AcidHCID 5356789OleylamineHCID 6326970Selenium2회

생성물 1

HCID 99411Di-n-octylphosphinic acid

시약·촉매·용매 5

HCID 887Methanol용매HCID 1140Toluene용매HCID 6342Acetonitrile용매HCID 82171-Octadecene용매2회HCID 13387N-methyl-2-pyrrolidone용매2회

실험 절차

Materials. 1-methyl-2-pyrrolidinone (99.5%, Aldrich), 1-octadecene (90%, Aldrich), acetonitrile (99.9%, Fisher Chemical), BiCl3 (99.999%, Strem), CdO (99.5%, Aldrich), diphenyl ether (99%, Aldrich), methanol (ACS grade, VWR), oleic acid (90%, Aldrich), oleylamine (70% Aldrich), selenium (99.99%, Strem), trioctylphosphine (90%, Aldrich), trioctylphosphine oxide (99%, Strem), toluene (ACS grade, VWR). 0.1M Se-ODE was prepared by dissolving selenium powder in 1-octadecene at 180° C. for 5 hr under inert atmosphere according to the procedure by Bullen et al. [42]; trioctylphosphine oxide (TOPO) was recrystallized from acetonitrile prior to use; di-n-octylphosphinic acid (DOPA) was synthesized according to the procedure reported by Wang et al. [1], a stock suspension of 2 mM BiCl3 in NMP was prepared in advance.

후처리

  1. custom0.1M Se-ODE was prepared
  2. customtrioctylphosphine oxide (TOPO) was recrystallized from acetonitrile
  3. customwas prepared in advance

출처 및 근거

ORD 기록
ord-cb7f6477f1344635a0b17cb21d123fc0
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09306110B2

연결된 노트

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