Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) → HCID 21023949、化合物

HRID 1446641ノート

反応式

HRID 1446641 の反応式
C1(C)C=CC(S([O-])(=O)=O)=CC=1.[NH+]1C=CC=CC=1.C(OC([O:23][CH:24]1[CH2:36][CH2:35][C:34]([O:38]C(OCC)C)([CH3:37])[CH:33]([O:44][C:45](=[O:53])[CH2:46][N:47]2[CH2:52][CH2:51][O:50][CH2:49][CH2:48]2)[CH:32]=[CH:31][CH:30]([CH3:54])[CH:29](/[C:55](/[CH3:76])=[CH:56]/[CH:57]=[CH:58]/[CH:59]([CH3:75])[CH2:60][CH:61]2[O:74][CH:62]2[CH:63]([CH3:73])[CH:64]([O:67]C(OCC)C)[CH2:65][CH3:66])[O:28][C:26](=[O:27])[CH2:25]1)C)C>CO>[OH:23][CH:24]1[CH2:36][CH2:35][C:34]([OH:38])([CH3:37])[CH:33]([O:44][C:45](=[O:53])[CH2:46][N:47]2[CH2:48][CH2:49][O:50][CH2:51][CH2:52]2)[CH:32]=[CH:31][CH:30]([CH3:54])[CH:29](/[C:55](/[CH3:76])=[CH:56]/[CH:57]=[CH:58]/[CH:59]([CH3:75])[CH2:60][CH:61]2[O:74][CH:62]2[CH:63]([CH3:73])[CH:64]([OH:67])[CH2:65][CH3:66])[O:28][C:26](=[O:27])[CH2:25]1

参加物

4

反応物 2

HCID 466102Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)HCID 21023946HCID 21023946、化合物

生成物 1

HCID 21023949HCID 21023949、化合物収率 82%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Pyridinium p-toluenesulfonate (2.2 mg, 8.71 μmol) was added to a solution of (8E,12E,14E)-3,6,21-tri(1-ethoxyethoxy)-6,10,12,16,20-pentamethyl-7-(morpholin-4-yl)acetoxy-18,19-epoxytricosa-8,12,14-trien-11-olide (7.3 mg, 8.71 μmol) in methanol (1 mL), followed by stirring at room temperature overnight. The reaction solution was evaporated, and to the resulting residue were added ethyl acetate, water and a saturated sodium bicarbonate aqueous solution. The mixture was extracted with ethyl acetate, and the resulting organic layer was dried over anhydrous magnesium sulfate, filtered and then evaporated. The resulting residue was purified by thin layer chromatography (MERCK Silica gel 60 F254, 0.2 mm, developing solution; methanol-dichloromethane=1:19) to obtain the title compound (4.4 mg, 82%) as a colorless oil.

後処理

  1. customThe reaction solution was evaporated
  2. additionto the resulting residue were added ethyl acetate, water
  3. extractionThe mixture was extracted with ethyl acetate
  4. dry with materialthe resulting organic layer was dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customevaporated
  7. customThe resulting residue was purified by thin layer chromatography (MERCK Silica gel 60 F254, 0.2 mm, developing solution; methanol-dichloromethane=1:19)

出典と根拠

ORDレコード
ord-fd592f6193554f52a52b5e6b27d4bd79
出典データセット
uspto-grants-2010_02
特許番号
US07667052B2

反応ノート

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