참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Trifluoroacetic acid | HCID 6422 | — |
| 반응물 | 2-(Benzyloxy)-4-((4-fluorophenyl)ethynyl)-5-(methoxymethoxy)pyridine | HCID 67217605 | — |
| 용매 | 1,1-Dichloroethane | HCID 6365 | — |
| 생성물 | 6-(Benzyloxy)-4-((4-fluorophenyl)ethynyl)pyridin-3-ol | HCID 67217295 | 100% |
반응 단계
Trifluoroacetic acid (0.95 mL, 12.4 mmol) was added to a stirring solution of 2-(benzyloxy)-4-((4-fluorophenyl)ethynyl)-5-(methoxymethoxy)pyridine (450 mg, 1.24 mmol) in dichloroethane (5 mL) at room temperature. It was allowed to stir for 5 hours and then concentrated to dryness to give 6-(benzyloxy)-4-((4-fluorophenyl)ethynyl)pyridin-3-ol (395 mg, 1.24 mmol, 100% yield) consistent by LCMS. LC-MS retention time: 2.49 min; m/z (MH+): 320. LC data was recorded on a Shimadzu LC-10AS liquid chromatograph equipped with a Waters SunFire 5u C18 4.6×50 mm column using a SPD-10AV UV-Vis detector at a detector wave length of 220 nM. The elution conditions employed a flow rate of 5 ml/min, a gradient of 100% solvent A/0% solvent B to 0% solvent A/100% solvent B, a gradient time of 3 min, a hold time of 1 min, and an analysis time of 4 min where solvent A was 10% acetonitrile/90% H2O/0.1% trifluoroacetic acid and solvent B was 10% H2O/90% acetonitrile/0.1% trifluoroacetic acid. MS data was determined using a Micromass Platform for LC in electrospray mode.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08536338B2 |
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| 출처 데이터셋 | uspto-grants-2013_09 |
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| ORD ID | ord-377e2992b15f4742b2a63460950ce727 |
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| 출처 메모 | uspto-grants-2013_09 |
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