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Hydrochloric Acid → HCID 57747224, 화합물

HRID 1163462
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HRID 1163462 반응식
[OH:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][C:3]=1[O:10][CH3:11].[I-].[Na+].C(=O)([O-])[O-].[K+].[K+].Br[CH2:21][C:22]([C:24]1[CH:29]=[C:28]([CH:30]2[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]2)[C:27]([OH:36])=[C:26]([CH:37]2[CH2:42][CH2:41][CH2:40][CH2:39][CH2:38]2)[CH:25]=1)=[O:23].Cl>C(OCC)(=O)C>[CH:30]1([C:28]2[CH:29]=[C:24]([C:22](=[O:23])[CH2:21][O:1][C:2]3[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][C:3]=3[O:10][CH3:11])[CH:25]=[C:26]([CH:37]3[CH2:38][CH2:39][CH2:40][CH2:41][CH2:42]3)[C:27]=2[OH:36])[CH2:31][CH2:32][CH2:33][CH2:34][CH2:35]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 1183VanillinHCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 87394924HCID 87394924, 화합물

생성물 1

HCID 57747224HCID 57747224, 화합물수율 30%

시약·촉매·용매 1

HCID 8857
Ethyl Acetate
용매

실험 절차

A mixture of 1.52 g (10 mmol) of 4-hydroxy-3-methoxy-benzaldehyde, 0.3 g (2.0 mmol) of sodium iodide and 3.05 g (22 mmol) of potassium carbonate in 80 ml of ethyl acetate is stirred for 30 minutes. Then 3.8 g (10 mmol) of 2-bromo-1-(4-hydroxy-3,5-di-cyclohexylphenyl)-ethanone is added and stirring at room temperature is continued for 16 hours. Then the mixture is acidified with 2N HCl and extracted with ethyl acetate. The combined extracts are washed with water, dried and evaporated. Crystallization of the crude product from dichloro-methane/di-isopropylether yields 1.35 g of compound 103, m.p. 163-164° C.

후처리

  1. stirringstirring at room temperature
  2. waitis continued for 16 hours
  3. extractionextracted with ethyl acetate
  4. washThe combined extracts are washed with water
  5. customdried
  6. customevaporated
  7. customCrystallization of the crude product from dichloro-methane/di-isopropylether

출처 및 근거

ORD 기록
ord-782d8c623d8b433c83e1f9ae8f5df1fb
출처 데이터셋
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07820865B2

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