Potassium Carbonate → HCID 57589084, 화합물

HRID 1782756노트

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HRID 1782756 반응식
Br[CH2:2][CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([O:11][CH2:12][CH2:13][CH2:14][CH2:15][O:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[CH:7][CH:6]=1.[CH:23]([C:25]1[CH:26]=[C:27]([CH:33]=[CH:34][C:35]=1[OH:36])[C:28]([O:30][CH2:31][CH3:32])=[O:29])=[O:24].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH:23]([C:25]1[CH:26]=[C:27]([CH:33]=[CH:34][C:35]=1[O:36][CH2:2][CH2:3][CH2:4][C:5]1[CH:10]=[CH:9][C:8]([O:11][CH2:12][CH2:13][CH2:14][CH2:15][O:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[CH:7][CH:6]=1)[C:28]([O:30][CH2:31][CH3:32])=[O:29])=[O:24]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 271759Ethyl 3-formyl-4-hydroxybenzoateHCID 574437531-(3-Bromopropyl)-4-(4-phenoxybutoxy)benzene

생성물 1

HCID 57589084HCID 57589084, 화합물수율 80.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
40 °C

실험 절차

1.37 g (3.76 mmol) of 1-(3-bromopropyl)-4-(4-phenoxybutoxy)benzene, 0.79 g (3.76 mmol) of ethyl 3-formyl-4-hydroxybenzoate [CAS No. 82304-99-2] and 0.78 g (5.64 mmol) of potassium carbonate are dissolved in 20 ml of DMF, and the mixture is stirred at 40° C. for 16 hours. It is then concentrated, and the residue is taken up in 200 ml of water and extracted with dichloromethane (three times 100 ml). The combined organic phases are dried (sodium sulphate) and concentrated, and the crude product is purified by chromatography on silica gel (mobile phase gradient cyclohexane-->cyclohexane/ethyl acetate 5:1). 1.45 g of product are obtained.

후처리

  1. concentrationIt is then concentrated
  2. extractionextracted with dichloromethane (three times 100 ml)
  3. dry with materialThe combined organic phases are dried (sodium sulphate)
  4. concentrationconcentrated
  5. customthe crude product is purified by chromatography on silica gel (mobile phase gradient cyclohexane-->cyclohexane/ethyl acetate 5:1)

출처 및 근거

ORD 기록
ord-6ed629ecbb44458f9e3723db1e524f27
출처 데이터셋
uspto-grants-2009_03
특허 번호
US07498460B2

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