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

HRID 1795695노트

반응식

HRID 1795695 반응식
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

참가 물질

4

반응물 2

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

생성물 1

HCID 58619154HCID 58619154, 화합물수율 68.5%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-aebfc05e2e83408aacbd17777875445c
출처 데이터셋
uspto-grants-2006_04
특허 번호
US07026352B1

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