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Dichloromethane → HCID 24812203, 화합물

HRID 1945463
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인쇄 미리보기

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HRID 1945463 반응식
[C:1]12([C:11]3[CH:22]=[CH:21][C:14]([O:15][CH2:16][CH2:17]C(O)=O)=[CH:13][CH:12]=3)[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[CH2:2]1)[CH2:8]2.[CH3:23][O:24][C:25](=[O:34])[C:26]1[CH:31]=[CH:30][C:29]([OH:32])=[C:28]([NH2:33])[CH:27]=1.ClCCl.[OH-].[Na+]>C[Si](OP(=O)=O)(C)C>[CH3:23][O:24][C:25]([C:26]1[CH:31]=[CH:30][C:29]2[O:32][C:17]([CH2:16][O:15][C:14]3[CH:13]=[CH:12][C:11]([C:1]45[CH2:10][CH:5]6[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]6)[CH2:2]4)[CH2:8]5)=[CH:22][CH:21]=3)=[N:33][C:28]=2[CH:27]=1)=[O:34]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 10815Methyl 3-amino-4-hydroxybenzoateHCID 14798Sodium HydroxideHCID 16772355(4-Adamantan-1-yl-phenoxymethyl)acetic acid

생성물 1

HCID 24812203HCID 24812203, 화합물수율 64.1%

시약·촉매·용매 1

HCID 16133246
Trimethyl(phosphooxy)silane
용매

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온도
140 °C

실험 절차

A mixture of (4-adamantan-1-yl-phenoxymethyl)-acetic acid (200.0 mg, 0.70 mmol) and 3-amino-4-hydroxy-benzoic acid methyl ester (164.3 mg, 0.98 mmol) in PPSE (3 mL) was heated at 140° C. for 2 h. At the end of the reaction period, the mixture was taken to dichloromethane and neutralized with 1 N NaOH solution. The organic layer was separated and the aqueous solution extracted with dichloromethane. The combined extracts were dried over anhydrous MgSO4, filtered and the solvent was removed with rotary evaporator under reduced pressure. The residue was purified by flash chromatography (n-Hexane:EtoAc:MeOH=6:3:1) to afford 2-(4-adamantan-1-yl-phenoxymethyl)-benzoxazole-5-carboxylic acid methyl ester as a white solid (187.3 mg, 64.1% yield).

후처리

  1. customAt the end of the reaction period
  2. customThe organic layer was separated
  3. extractionthe aqueous solution extracted with dichloromethane
  4. dry with materialThe combined extracts were dried over anhydrous MgSO4
  5. filtrationfiltered
  6. customthe solvent was removed with rotary evaporator under reduced pressure
  7. customThe residue was purified by flash chromatography (n-Hexane:EtoAc:MeOH=6:3:1)

출처 및 근거

ORD 기록
ord-c8c6abfa0e8642a8ae145363186a44ef
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08394799B2

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