Methanesulfonic Acid → 2,6-Diphenylphenoxyethyl acrylate

HRID 1506746

반응식

HRID 1506746 반응식
C(OC1C=CC(C(C2C=CC(OC(=O)C=C)=CC=2)(C2C=CC(OC(=O)C=C)=CC=2)C)=CC=1)(=O)C=C.[C:36]1([C:42]2[CH:51]=[CH:50][CH:49]=[C:48]([C:52]3[CH:57]=[CH:56][CH:55]=[CH:54][CH:53]=3)[C:43]=2[O:44][CH:45](O)[CH3:46])[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1.[C:58]([OH:62])(=[O:61])[CH:59]=[CH2:60].CS(O)(=O)=O>C1(C)C=CC=CC=1>[C:58]([O:62][CH2:46][CH2:45][O:44][C:43]1[C:48]([C:52]2[CH:57]=[CH:56][CH:55]=[CH:54][CH:53]=2)=[CH:49][CH:50]=[CH:51][C:42]=1[C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1)(=[O:61])[CH:59]=[CH2:60]

참가 물질

6

반응물 4

HCID 6395Methanesulfonic AcidHCID 6581Acrylic AcidHCID 11568972Acrylic acid 4-[1,1-bis-(4-acryloyloxy-phenyl)-ethyl]-phenyl esterHCID 689761212,6-Diphenylphenoxyethanol

생성물 1

HCID 689780572,6-Diphenylphenoxyethyl acrylate

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a 50 ml 1 neck round bottom equipped with a dean stark trap was added 2,6-diphenylphenoxyethanol (5 g, 1 eq), toluene (21 ml), acrylic acid (2.7 g, 2.2 eq), methane sulfonic acid (0.3 g, 0.18 eq), Prostab 5198 (0.003 g) and heated to reflux. After 3 hours the reaction was complete. The reaction was washed with 20 ml sodium carbonate and 20 ml sodium chloride brine. The toluene mixture was filtered through thin layer of silica gel and eluted with 30 ml toluene. The filtrate was treated with the “Prostab 5198” (0.003 g) and concentrated invacuo to recover a viscous oil. >97% by GC. RI=1.6062 at 25° C.

후처리

  1. temperatureheated to reflux
  2. washThe reaction was washed with 20 ml sodium carbonate and 20 ml sodium chloride brine
  3. filtrationThe toluene mixture was filtered through thin layer of silica gel
  4. washeluted with 30 ml toluene
  5. additionThe filtrate was treated with the “Prostab 5198” (0.003 g)
  6. concentrationconcentrated invacuo
  7. customto recover a viscous oil
  8. customat 25° C.

출처 및 근거

ORD 기록
ord-e9b2757679e64b06b69c14ecf0651ed8
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09221743B2

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