Acetonitrile → 1-O-(2,4,8,10-Tetra-tert-butyl-dibenzo[d,f][1,3,2]dioxaphosphepin-6-yl)-2,2'-methylenebis-(4,6-di-tert-butylphenol)

HRID 487033

反応式

HRID 487033 の反応式
[CH2:1]([C:17]1[CH:22]=[C:21]([C:23]([CH3:26])([CH3:25])[CH3:24])[CH:20]=[C:19]([C:27]([CH3:30])([CH3:29])[CH3:28])[C:18]=1[OH:31])[C:2]1[CH:7]=[C:6]([C:8]([CH3:11])([CH3:10])[CH3:9])[CH:5]=[C:4]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:3]=1[OH:16].C(N(CC)CC)C.Cl[C:40]1[C:41]([C:67]([CH3:70])([CH3:69])[CH3:68])=[CH:42][C:43]2[C:49]3[CH:50]=[C:51]([C:58]([CH3:61])([CH3:60])[CH3:59])[CH:52]=[C:53]([C:54]([CH3:57])([CH3:56])[CH3:55])[C:48]=3[O:47][PH:46][O:45][C:44]=2[C:62]=1[C:63]([CH3:66])([CH3:65])[CH3:64].C(#N)C>C1(C)C=CC=CC=1>[C:58]([C:51]1[CH:52]=[C:53]([C:54]([CH3:57])([CH3:56])[CH3:55])[C:48]2[O:47][P:46]([O:31][C:18]3[C:19]([C:27]([CH3:30])([CH3:29])[CH3:28])=[CH:20][C:21]([C:23]([CH3:26])([CH3:25])[CH3:24])=[CH:22][C:17]=3[CH2:1][C:2]3[CH:7]=[C:6]([C:8]([CH3:11])([CH3:9])[CH3:10])[CH:5]=[C:4]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:3]=3[OH:16])[O:45][C:44]3[C:62]([C:63]([CH3:65])([CH3:64])[CH3:66])=[CH:40][C:41]([C:67]([CH3:70])([CH3:69])[CH3:68])=[CH:42][C:43]=3[C:49]=2[CH:50]=1)([CH3:61])([CH3:60])[CH3:59]

参加物

6

反応物 4

HCID 6342AcetonitrileHCID 8471TriethylamineHCID 843912,2'-Methylenebis(4,6-di-tert-butylphenol)HCID 190964063-Chloro-2,4,8,10-tetra-tert-butyl-dibenzo[d,f][1,3,2]dioxaphosphepin

生成物 1

HCID 190964071-O-(2,4,8,10-Tetra-tert-butyl-dibenzo[d,f][1,3,2]dioxaphosphepin-6-yl)-2,2'-methylenebis-(4,6-di-tert-butylphenol)収率 85%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

Into a solution of 21.23 g (50 mmol) of 2,2'-methylenebis(4,6-di-tert-butylphenol) and 7 mL (50 mmol) of triethylamine in 200 mL of toluene is added dropwise a solution of 23.84 g (50 mmol) of 3-chloro-2,4,8,10-tetra-tert-butyl-dibenzo[d,f][1,3,2]dioxaphosphepin in 100 mL of toluene at ambient temperature. After 20 hours of stirring at ambient temperature, the reaction mass is filtered to remove triethylamine hydrochloride and the filtrate is concentrated in vacuo to give a brownish oil. Trituration of the crude oil with 200 mL of acetonitrile gives 36.65 g (85% yield) of a white solid: m.p.=195°-205° C.

後処理

  1. filtrationthe reaction mass is filtered
  2. customto remove triethylamine hydrochloride
  3. concentrationthe filtrate is concentrated in vacuo
  4. customto give a brownish oil

出典と根拠

ORDレコード
ord-28a6dfbc7a7345e7821328838a35d828
出典データセット
uspto-grants-1994_03
特許番号
US05292785

関連ノート

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