Triethylamine → HCID 86604547, 화합물

HRID 1446646노트

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HRID 1446646 반응식
ClC(O[C:5]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][CH:6]=1)=O.[CH2:14]([O:16][CH:17]([O:19][CH:20]1[CH2:32][CH2:31][C:30]([O:34][CH:35]([O:37][CH2:38][CH3:39])[CH3:36])([CH3:33])[CH:29]([OH:40])[CH:28]=[CH:27][CH:26]([CH3:41])[CH:25](/[C:42](/[CH3:63])=[CH:43]/[CH:44]=[CH:45]/[CH:46]([CH3:62])[CH2:47][CH:48]2[O:61][CH:49]2[CH:50]([CH3:60])[CH:51]([O:54][CH:55]([O:57][CH2:58][CH3:59])[CH3:56])[CH2:52][CH3:53])[O:24][C:22](=[O:23])[CH2:21]1)[CH3:18])[CH3:15].C(N(CC)CC)C.CN(C1C=CC=CN=1)C.[C:80](=O)([OH:82])[O-:81].[Na+]>ClCCl.O.C(OCC)(=O)C>[CH2:14]([O:16][CH:17]([O:19][CH:20]1[CH2:32][CH2:31][C:30]([O:34][CH:35]([O:37][CH2:38][CH3:39])[CH3:36])([CH3:33])[CH:29]([O:40][C:5]2[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][CH:6]=2)[CH:28]=[CH:27][CH:26]([CH3:41])[CH:25](/[C:42](/[CH3:63])=[CH:43]/[CH:44]=[CH:45]/[CH:46]([CH3:62])[CH2:47][CH:48]2[O:61][CH:49]2[CH:50]([CH3:60])[CH:51]([O:54][CH:55]([O:57][CH2:58][CH3:59])[CH3:56])[CH2:52][CH3:53])[O:24][C:22](=[O:23])[CH:21]1[C:80]([OH:82])=[O:81])[CH3:18])[CH3:15]

참가 물질

9

반응물 5

HCID 8471TriethylamineHCID 218852-DimethylaminopyridineHCID 821294-Nitrophenyl chloroformateHCID 516892Sodium BicarbonateHCID 21023947(8E,12E,14E)-3,6,21-Tri(1-ethoxyethoxy)-7-hydroxy-6,10,12,16,20-pentamethyl-18,19-epoxytricosa-8,12,14-trien-11-olide

생성물 1

HCID 86604547HCID 86604547, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 6344Dichloromethane용매2회HCID 8857Ethyl Acetate용매

실험 절차

A solution of 4-nitrophenyl chloroformate (62 mg, 300 μmol) in dichloromethane (2.5 mL) was added dropwise into a solution of (8E,12E,14E)-3,6,21-tri(1-ethoxyethoxy)-7-hydroxy-6,10,12,16,20-pentamethyl-18,19-epoxytricosa-8,12,14-trien-11-olide (35 mg, 49.2 μmol), triethylamine (61 mg, 600 μmol) and dimethylaminopyridine (4 mg, 30 μmol) in dichloromethane (2.5 mL), followed by stirring at room temperature for 2.5 hours under nitrogen atmosphere. Ethyl acetate, water and saturated sodium bicarbonate aqueous solution were added to the reaction mixture, and the mixture was extracted with ethyl acetate, then the organic layer was washed with water. The resulting organic layer was dried over anhydrous magnesium sulfate, filtered and then evaporated to give the title crude compound (92.2 mg) as a yellow oil. This was used for the following reaction without purification.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washthe organic layer was washed with water
  3. dry with materialThe resulting organic layer was dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. customevaporated

출처 및 근거

ORD 기록
ord-b4785036456d42debeffea309a35afb9
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07667052B2

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