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Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) → HCID 21024034, 화합물

HRID 1446648
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HRID 1446648 반응식
C1(C)C=CC(S([O-])(=O)=O)=CC=1.[NH+]1C=CC=CC=1.[C:18]([O:21][CH:22]1[C:23]([O:65]C(OCC)C)([CH3:64])[CH2:24][CH2:25][CH:26]([O:58]C(OCC)C)[CH2:27][C:28]([O:30][CH:31](/[C:36](/[CH3:57])=[CH:37]/[CH:38]=[CH:39]/[CH:40]([CH3:56])[CH2:41][CH:42]2[O:55][CH:43]2[CH:44]([CH3:54])[CH:45]([O:48]C(OCC)C)[CH2:46][CH3:47])[CH:32]([CH3:35])[CH:33]=[CH:34]1)=[O:29])(=[O:20])[NH2:19]>CO>[C:18]([O:21][CH:22]1[C:23]([OH:65])([CH3:64])[CH2:24][CH2:25][CH:26]([OH:58])[CH2:27][C:28]([O:30][CH:31](/[C:36](/[CH3:57])=[CH:37]/[CH:38]=[CH:39]/[CH:40]([CH3:56])[CH2:41][CH:42]2[O:55][CH:43]2[CH:44]([CH3:54])[CH:45]([OH:48])[CH2:46][CH3:47])[CH:32]([CH3:35])[CH:33]=[CH:34]1)=[O:29])(=[O:20])[NH2:19]
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참가 물질

4

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HCID 466102Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)HCID 21024033(8E,12E,14E)-7-Carbamoyloxy-3,6,21-tri(1-ethoxyethoxy)-6,10,12,16,20-pentamethyl-18,19-epoxytricosa-8,12,14-trien-11-olide

생성물 1

HCID 21024034HCID 21024034, 화합물수율 74.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Pyridinium p-toluenesulfonate (1.2 mg, 4.8 μmol) was added to a solution of (8E,12E,14E)-7-carbamoyloxy-3,6,21-tri(1-ethoxyethoxy)-6,10,12,16,20-pentamethyl-18,19-epoxytricosa-8,12,14-trien-11-olide (3.6 mg, 4.77 μmol) in methanol (1 mL), followed by stirring at room temperature for 3 hours. The reaction mixture 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; methanol-dichloromethane, 1:29) to give the title compound (1.9 mg, 74%) as a colorless oil.

후처리

  1. customThe reaction mixture 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; methanol-dichloromethane, 1:29)

출처 및 근거

ORD 기록
ord-36e688c83b25421a8b159a93aec715c1
출처 데이터셋
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07667052B2

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