Methanesulfonic Acid → 2,6-Diphenylphenoxyethyl acrylate

HRID 539433

反応式

HRID 539433 の反応式
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]

参加物

6

反応物 4

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

生成物 1

HCID 689780572,6-Diphenylphenoxyethyl acrylate

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-ac5f5e343a9943e7a4e8baf1a5a5c939
出典データセット
uspto-grants-2014_10
特許番号
US08871315B2

関連ノート

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