Hydrochloric Acid → (R)-2-Amino-2-(5-fluoropyridin-2-yl)ethanol hydrochloride

HRID 450372노트

반응식

HRID 450372 반응식
[Si]([O:8][CH2:9][C@H:10]([NH:18]S(C(C)(C)C)=O)[C:11]1[CH:16]=[CH:15][C:14]([F:17])=[CH:13][N:12]=1)(C(C)(C)C)(C)C.[ClH:25]>CO>[ClH:25].[NH2:18][C@H:10]([C:11]1[CH:16]=[CH:15][C:14]([F:17])=[CH:13][N:12]=1)[CH2:9][OH:8]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 68479628(RS)-N-[(1R)-2-{[tert-Butyl(dimethyl)silyl]oxy}-1-(5-fluoropyridin-2-yl)ethyl]-2-methylpropane-2-sulfinamide2회

생성물 1

HCID 68482269(R)-2-Amino-2-(5-fluoropyridin-2-yl)ethanol hydrochloride수율 98.8%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of (RS)—N-[(1R)-2-{[tert-butyl(dimethyl)silyl]oxy}-1-(5-fluoropyridin-2-yl)ethyl]-2-methylpropane-2-sulfinamide (Intermediate 22, 1.13 g, 3.02 mmol) in MeOH (15 ml) was added hydrochloric acid (4 M in dioxane, 3.02 ml, 12.08 mol) at 0° C. and the mixture was stirred for 15 minutes and was concentrated. The mixture was triturated from hexanes to provide the title salt (575 mg). The product is highly hygroscopic. 1H NMR (300 MHz, DMSO-d6) δ ppm 8.62 (s, 1H) 8.55 (s, 2H) 7.76-7.93 (m, 1H) 7.65 (dd, J=8.29, 4.52 Hz, 1H) 4.43 (d, J=4.52 Hz, 1H) 3.77 (s, 2H).

후처리

  1. concentrationwas concentrated
  2. customThe mixture was triturated from hexanes

출처 및 근거

ORD 기록
ord-9356412212ae47449074dc5f80a317c9
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486966B2

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