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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Potassium Carbonate → 2,3-dihydro-2,2-bis(pent-4-enyl)-8-propyl-7-[3-[(5,6,7,8-tetrahydro-1-naphthalenyl)oxy]propoxy]-4H-1-benzopyran-4-one

HRID 2371647
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HRID 2371647 반응식
[CH2:1]([C:6]1([CH2:21][CH2:22][CH2:23][CH:24]=[CH2:25])[CH2:11][C:10](=[O:12])[C:9]2[CH:13]=[CH:14][C:15]([OH:20])=[C:16]([CH2:17][CH2:18][CH3:19])[C:8]=2[O:7]1)[CH2:2][CH2:3][CH:4]=[CH2:5].[C:26]1([O:36][CH2:37][CH2:38][CH2:39]Br)[C:35]2[CH2:34][CH2:33][CH2:32][CH2:31][C:30]=2[CH:29]=[CH:28][CH:27]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH2:21]([C:6]1([CH2:1][CH2:2][CH2:3][CH:4]=[CH2:5])[CH2:11][C:10](=[O:12])[C:9]2[CH:13]=[CH:14][C:15]([O:20][CH2:39][CH2:38][CH2:37][O:36][C:26]3[C:35]4[CH2:34][CH2:33][CH2:32][CH2:31][C:30]=4[CH:29]=[CH:28][CH:27]=3)=[C:16]([CH2:17][CH2:18][CH3:19])[C:8]=2[O:7]1)[CH2:22][CH2:23][CH:24]=[CH2:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 144059475-(3-Bromopropoxy)-1,2,3,4-tetrahydronaphthaleneHCID 151574722,3-dihydro-2,2-bis(pent-4-enyl)-8-propyl-7-hydroxy-4H-1-benzopyran-4-one

생성물 1

HCID 151574732,3-dihydro-2,2-bis(pent-4-enyl)-8-propyl-7-[3-[(5,6,7,8-tetrahydro-1-naphthalenyl)oxy]propoxy]-4H-1-benzopyran-4-one수율 82.7%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

To a solution of 3.0 g (9.55 mmol) of the title product of Example 69 and 4.01 g (11 mmol) of the title product of Example 12 in 56 ml of dry dimethylformamide (DMF) was added 2.77 g (20.1 mmol) of anhydrous potassium carbonate. The resulting mixture was stirred overnight at room temperature. The solvent was removed in vacuo, and the residue was partitioned between ethyl acetate and 3N hydrochloric acid. The aqueous layer was further extracted with two portions of ethyl acetate. The combined organic extracts were washed with water and with brine, dried over magnesium sulfate, filtered, and the solvent removed under reduced pressure. Chromatography of the residue over silica gel, using 10% ethyl acetate/hexane as eluent, gave the title compound (4.19 g) as an oil.

후처리

  1. customThe solvent was removed in vacuo
  2. customthe residue was partitioned between ethyl acetate and 3N hydrochloric acid
  3. extractionThe aqueous layer was further extracted with two portions of ethyl acetate
  4. washThe combined organic extracts were washed with water and with brine
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. customthe solvent removed under reduced pressure

출처 및 근거

ORD 기록
ord-7ea2eed87e164336a293e542615fd537
출처 데이터셋
uspto-grants-1992_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05093353

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