Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) → HCID 21024032、化合物

HRID 1795693ノート

反応式

HRID 1795693 の反応式
C1(C)C=CC(S([O-])(=O)=O)=CC=1.[NH+]1C=CC=CC=1.[C:18]([O:26][CH:27]1[C:28]([O:70]C(OCC)C)([CH3:69])[CH2:29][CH2:30][CH:31]([O:63]C(OCC)C)[CH2:32][C:33]([O:35][CH:36](/[C:41](/[CH3:62])=[CH:42]/[CH:43]=[CH:44]/[CH:45]([CH3:61])[CH2:46][CH:47]2[O:60][CH:48]2[CH:49]([CH3:59])[CH:50]([O:53]C(OCC)C)[CH2:51][CH3:52])[CH:37]([CH3:40])[CH:38]=[CH:39]1)=[O:34])(=[O:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>CO>[C:18]([O:26][CH:27]1[C:28]([OH:70])([CH3:69])[CH2:29][CH2:30][CH:31]([OH:63])[CH2:32][C:33]([O:35][CH:36](/[C:41](/[CH3:62])=[CH:42]/[CH:43]=[CH:44]/[CH:45]([CH3:61])[CH2:46][CH:47]2[O:60][CH:48]2[CH:49]([CH3:59])[CH:50]([OH:53])[CH2:51][CH3:52])[CH:37]([CH3:40])[CH:38]=[CH:39]1)=[O:34])(=[O:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1

参加物

4

反応物 2

HCID 466102Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)HCID 21024031HCID 21024031、化合物

生成物 1

HCID 21024032HCID 21024032、化合物収率 74%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Pyridinium p-toluenesulfonate (2 mg, 7.5 μmol) was added to a solution of (8E,12E,14E)-7-benzoyloxy-3,6,21-tri(1-ethoxyethoxy)-6,10,12,16,20-pentamethyl-18,19-epoxytricosa-8,12,14-trien-11-olide (6.1 mg, 7.48 μmol) in methanol (1 mL), followed by stirring at room temperature for one hour. The reaction solution was evaporated, ethyl acetate, water and a saturated sodium bicarbonate aqueous solution were added to the resulting residue, and the mixture was extracted with ethyl acetate. 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 acetatehexane=2:1) to obtain the title compound (3.3 mg, 74%) as a colorless oil.

後処理

  1. customThe reaction solution was evaporated
  2. additionethyl acetate, water and a saturated sodium bicarbonate aqueous solution were added to the resulting residue
  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 acetatehexane=2:1)

出典と根拠

ORDレコード
ord-e0452191cbcf44bda2e94d1c23a5b64f
出典データセット
uspto-grants-2006_04
特許番号
US07026352B1

反応ノート

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