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Imidazole → HCID 22709782, 화합물

HRID 352840
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HRID 352840 반응식
[OH:1][CH2:2][CH:3]1[CH2:12][CH2:11][C:10]2[C:5](=[CH:6][CH:7]=[C:8]([C:13]([O:15][CH3:16])=[O:14])[CH:9]=2)[CH2:4]1.N1C=CN=C1.[Si:22](Cl)([C:25]([CH3:28])([CH3:27])[CH3:26])([CH3:24])[CH3:23].CO>CN(C)C=O>[Si:22]([O:1][CH2:2][CH:3]1[CH2:12][CH2:11][C:10]2[C:5](=[CH:6][CH:7]=[C:8]([C:13]([O:15][CH3:16])=[O:14])[CH:9]=2)[CH2:4]1)([C:25]([CH3:28])([CH3:27])[CH3:26])([CH3:24])[CH3:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 795ImidazoleHCID 887MethanolHCID 28928tert-Butyldimethylsilyl chlorideHCID 13851838Methyl 6-hydroxymethyl-5,6,7,8-tetrahydro-2-naphthalenecarboxylate

생성물 1

HCID 22709782HCID 22709782, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

In N,N-dimethylformamide (5 ml), (2RS)-2-hydroxymethyl-6-methoxycarbonyl-1,2,3,4-tetrahydronaphthalene (1.71 g) was dissolved. To the resulting solution, imidazole (0.81 g) and tert-butyldimethylsilyl chloride (1.81 g) were added under ice cooling, followed by stirring at room temperature for 14 hours. After the addition of methanol, the mixture was concentrated under reduced pressure. The concentrate was diluted with ethyl acetate, washed with water and then dried over anhydrous sodium sulfate. The residue obtained by distilling off the solvent under reduced pressure was purified by chromatography (hexane:ethyl acetate=50:1), whereby a pale yellow solid (2.20 g, 85%) was obtained.

후처리

  1. concentrationthe mixture was concentrated under reduced pressure
  2. additionThe concentrate was diluted with ethyl acetate
  3. washwashed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe residue obtained
  6. distillationby distilling off the solvent under reduced pressure
  7. customwas purified by chromatography (hexane:ethyl acetate=50:1), whereby a pale yellow solid (2.20 g, 85%)
  8. customwas obtained

출처 및 근거

ORD 기록
ord-fd786f63f7e44a26afd35d4bafa85c7c
출처 데이터셋
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06747023B1

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