Diphenyl Ether → Di-n-octylphosphinic acid

HRID 625206

反応式

HRID 625206 の反応式
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]

参加物

12

反応物 6

HCID 7583Diphenyl EtherHCID 20851TrioctylphosphineHCID 65577Trioctylphosphine oxideHCID 445639Oleic AcidHCID 5356789OleylamineHCID 6326970Selenium2 回

生成物 1

HCID 99411Di-n-octylphosphinic acid

試薬・触媒・溶媒 5

HCID 887Methanol溶媒HCID 1140Toluene溶媒HCID 6342Acetonitrile溶媒HCID 82171-Octadecene溶媒2 回HCID 13387N-methyl-2-pyrrolidone溶媒2 回

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-6e78a7dff33e47fba556385f7ba7ed90
出典データセット
uspto-grants-2016_04
特許番号
US09306110B2

関連ノート

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