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

HRID 1446643노트

반응식

HRID 1446643 반응식
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

참가 물질

4

반응물 2

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

생성물 1

HCID 21024032HCID 21024032, 화합물수율 74%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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 acetate-hexane=2:1) to obtain the title compound (3.3 mg, 74%) as a colorless oil.

후처리

  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 acetate-hexane=2:1)

출처 및 근거

ORD 기록
ord-6dbb1e6332ca488785453759934638c3
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07667052B2

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