Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) → HCID 58619154、化合物

HRID 1446645ノート

反応式

HRID 1446645 の反応式
C1(C)C=CC(S([O-])(=O)=O)=CC=1.[NH+]1C=CC=CC=1.C(OC([O:23][C:24]1([CH3:61])[CH:36]([OH:37])[CH:35]=[CH:34][CH:33]([CH3:38])[CH:32](/[C:39](/[CH3:60])=[CH:40]/[CH:41]=[CH:42]/[CH:43]([CH3:59])[CH2:44][CH:45]2[O:58][CH:46]2[CH:47]([CH3:57])[CH:48]([O:51]C(OCC)C)[CH2:49][CH3:50])[O:31][C:29](=[O:30])[CH:28]=[CH:27][CH2:26][CH2:25]1)C)C>CO>[OH:23][C:24]1([CH3:61])[CH:36]([OH:37])[CH:35]=[CH:34][CH:33]([CH3:38])[CH:32](/[C:39](/[CH3:60])=[CH:40]/[CH:41]=[CH:42]/[CH:43]([CH3:59])[CH2:44][CH:45]2[O:58][CH:46]2[CH:47]([CH3:57])[CH:48]([OH:51])[CH2:49][CH3:50])[O:31][C:29](=[O:30])[CH:28]=[CH:27][CH2:26][CH2:25]1

参加物

4

反応物 2

HCID 466102Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)HCID 86604546HCID 86604546、化合物

生成物 1

HCID 58619154HCID 58619154、化合物収率 68.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Pyridinium p-toluenesulfonate (2 mg, 7.7 μmol) was added to a solution of (2Z,8E,12E,14E)-6,21-di(1-ethoxyethoxy)-7-hydroxy-6,10,12,16,20-pentamethyl-18,19-epoxytricosa-2,8,12,14-tetraen-11-olide (6.3 mg, 10.1 μmol) in methanol (1.5 mL), followed by stirring at room temperature for one hour. 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; ethyl acetate-hexane=4:3) to obtain the title compound (3.3 mg, 68%) 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; ethyl acetate-hexane=4:3)

出典と根拠

ORDレコード
ord-042ca3dd88a94f7a90c9a4db35e7224a
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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