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

반응식

HRID 487033 반응식
[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]

참가 물질

6

반응물 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

생성물 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)수율 85%

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-28a6dfbc7a7345e7821328838a35d828
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05292785

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