Diphenyl Ether → Di-n-octylphosphinic acid

HRID 625203

반응식

HRID 625203 반응식
C=CCCCCCCCCCCCCCCCC.C1([O:25]C2C=CC=CC=2)C=CC=CC=1.C(O)(=O)CCCCCCC/C=C\CCCCCCCC.C(N)CCCCCCC/C=C\CCCCCCCC.[Se].C([P:80](=[O:97])([CH2:89][CH2:90][CH2:91][CH2:92][CH2:93][CH2:94][CH2:95][CH3:96])[CH2:81][CH2:82][CH2:83][CH2:84][CH2:85][CH2:86][CH2:87][CH3:88])CCCCCCC>C(P(CCCCCCCC)CCCCCCCC)CCCCCCC.CN1C(=O)CCC1.C1(C)C=CC=CC=1.CO.C(#N)C>[CH2:89]([P:80]([CH2:81][CH2:82][CH2:83][CH2:84][CH2:85][CH2:86][CH2:87][CH3:88])(=[O:97])[OH:25])[CH2:90][CH2:91][CH2:92][CH2:93][CH2:94][CH2:95][CH3:96]

참가 물질

12

반응물 6

HCID 7583Diphenyl EtherHCID 82171-OctadeceneHCID 65577Trioctylphosphine oxideHCID 445639Oleic AcidHCID 5356789OleylamineHCID 6326970Selenium2회

생성물 1

HCID 99411Di-n-octylphosphinic acid

시약·촉매·용매 5

HCID 887Methanol용매HCID 1140Toluene용매HCID 6342Acetonitrile용매HCID 13387N-methyl-2-pyrrolidone용매2회HCID 20851Trioctylphosphine용매2회

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). 1M TOP-Se was prepared by dissolving selenium powder in trioctylphosphine under inert atmosphere; 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. custom1M TOP-Se was prepared
  2. customtrioctylphosphine oxide (TOPO) was recrystallized from acetonitrile
  3. customwas prepared in advance

출처 및 근거

ORD 기록
ord-d148e86f3f324da9951be3659285ba16
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09306110B2

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