Water → HCID 21023946, 화합물

HRID 1446640노트

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HRID 1446640 반응식
[NH:1]1[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.Cl[CH2:8][C:9]([O:11][CH:12]1[C:13]([O:55][CH:56]([O:58][CH2:59][CH3:60])[CH3:57])([CH3:54])[CH2:14][CH2:15][CH:16]([O:48][CH:49]([O:51][CH2:52][CH3:53])[CH3:50])[CH2:17][C:18]([O:20][CH:21](/[C:26](/[CH3:47])=[CH:27]/[CH:28]=[CH:29]/[CH:30]([CH3:46])[CH2:31][CH:32]2[O:45][CH:33]2[CH:34]([CH3:44])[CH:35]([O:38][CH:39]([O:41][CH2:42][CH3:43])[CH3:40])[CH2:36][CH3:37])[CH:22]([CH3:25])[CH:23]=[CH:24]1)=[O:19])=[O:10].C(OCC)(=O)C.O>CN(C)C=O>[CH2:52]([O:51][CH:49]([O:48][CH:16]1[CH2:15][CH2:14][C:13]([O:55][CH:56]([O:58][CH2:59][CH3:60])[CH3:57])([CH3:54])[CH:12]([O:11][C:9](=[O:10])[CH2:8][N:1]2[CH2:6][CH2:5][O:4][CH2:3][CH2:2]2)[CH:24]=[CH:23][CH:22]([CH3:25])[CH:21](/[C:26](/[CH3:47])=[CH:27]/[CH:28]=[CH:29]/[CH:30]([CH3:46])[CH2:31][CH:32]2[O:45][CH:33]2[CH:34]([CH3:44])[CH:35]([O:38][CH:39]([O:41][CH2:42][CH3:43])[CH3:40])[CH2:36][CH3:37])[O:20][C:18](=[O:19])[CH2:17]1)[CH3:50])[CH3:53]

참가 물질

6

반응물 4

HCID 962WaterHCID 8083MorpholineHCID 8857Ethyl AcetateHCID 21024035HCID 21024035, 화합물

생성물 1

HCID 21023946HCID 21023946, 화합물수율 85%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
60 °C

실험 절차

Morpholine (9 mg, 0.103 mmol) was added to a solution of (8E,12E,14E)-7-chloroacetoxy-3,6,21-tri(1-ethoxyethoxy)-6,10,12,16,20-pentamethyl-18,19-epoxytricosa-8,12,14-trien-11-olide (8.1 mg, 10.3 μmol) in N,N-dimethylformamide (1 mL) at room temperature, followed by stirring at 60° C. for one hour. Ethyl acetate and water were added to the reaction solution, and the mixture was extracted with ethyl acetate, and the organic layer was washed with water. The resulting organic layer was dried over anhydrous magnesium sulfate, filtered and then evaporated. The resulting residue was purified by silica gel column chromatography (Kanto silica gel 60N, 40 to 50 μm; ethyl acetate-hexane=1:2 and 1:1, successively) to obtain the title compound (7.3 mg, 85%) as a colorless oil.

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
  6. customThe resulting residue was purified by silica gel column chromatography (Kanto silica gel 60N, 40 to 50 μm

출처 및 근거

ORD 기록
ord-14428ab15c70494a85bf6f9289ffae68
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07667052B2

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