Sodium Iodide → HCID 15341832, 화합물

HRID 1033650노트

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HRID 1033650 반응식
[OH:1][C:2]1[C:10]([CH2:11][CH:12]=[CH2:13])=[C:9]([OH:14])[CH:8]=[CH:7][C:3]=1[C:4]([NH2:6])=[O:5].Cl[CH2:16][CH2:17][CH2:18][O:19][C:20]1[C:21]([CH2:33][CH2:34][CH3:35])=[C:22]([CH:30]=[CH:31][CH:32]=1)[O:23][CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26].[I-].[Na+].C(=O)([O-])[O-].[K+].[K+]>C(OCC)(=O)C.CCCCCC.O.CN(C=O)C>[NH2:6][C:4]([C:3]1[CH:7]=[CH:8][C:9]([O:14][CH2:16][CH2:17][CH2:18][O:19][C:20]2[C:21]([CH2:33][CH2:34][CH3:35])=[C:22]([CH:30]=[CH:31][CH:32]=2)[O:23][CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26])=[C:10]([CH2:11][CH:12]=[CH2:13])[C:2]=1[OH:1])=[O:5]

참가 물질

8

반응물 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 15341803HCID 15341803, 화합물HCID 15341816HCID 15341816, 화합물

생성물 1

HCID 15341832HCID 15341832, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 21226206Ethyl acetate hexane용매

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온도
40 °C

실험 절차

2,4-Dihydroxy-3-(2-propenyl)benzamide(193 mg 1.0 mmol), ethyl [3-(3-chloropropoxy)-2-propylphenoxy]acetate(386 mg, 1.0 mmol), sodium iodide (276 mg, 2.0 mmol), and potassium carbonate (276 mg, 2.0 mmol) were added to 2.0 ml of DMF, and the reaction mixture was heated in an oil bath at 40° C. overnight. The temperature was raised to 60° C., and the reaction mixture was again heated overnight. The reaction mixture was poured into 15 ml of water and extracted three times with ethyl acetate. The combined extracts were washed twice with water, dried and filtered. The solvent was removed under vacuum to give the crude product as a solid. Chromatography of the crude product on silica gel with 50/50 ethyl acetate/hexane as eluant gave the product.

후처리

  1. temperatureThe temperature was raised to 60° C.
  2. extractionextracted three times with ethyl acetate
  3. washThe combined extracts were washed twice with water
  4. customdried
  5. filtrationfiltered
  6. customThe solvent was removed under vacuum
  7. customto give the crude product as a solid

출처 및 근거

ORD 기록
ord-2eacf1cf948c467c9bb18abac8e6475d
출처 데이터셋
uspto-grants-1994_05
특허 번호
US05310951

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