Hydrochloric Acid → HCID 58739076, 화합물

HRID 720278노트

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HRID 720278 반응식
C([O:3][C:4]([C:6]1[N:7]=[C:8]([N:16]2[CH2:21][CH2:20][CH2:19][CH2:18][S:17]2(=[O:23])=[O:22])[N:9]([CH3:15])[C:10](=[O:14])[C:11]=1[O:12][CH3:13])=[O:5])C.[OH-].[Na+].Cl>C(O)C>[O:23]=[S:17]1(=[O:22])[CH2:18][CH2:19][CH2:20][CH2:21][N:16]1[C:8]1[N:9]([CH3:15])[C:10](=[O:14])[C:11]([O:12][CH3:13])=[C:6]([C:4]([OH:5])=[O:3])[N:7]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 58739069HCID 58739069, 화합물

생성물 1

HCID 58739076HCID 58739076, 화합물수율 81%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 2-(1,1-dioxo-1λ6-[1,2]thiazinan-2-yl)-5-methoxy-1-methyl-6-oxo-1,6-dihydro-pyrimidine-4-carboxylic acid ethyl ester (0.180 g, 0.52 mmol) in 90% ethanol (10 ml) was treated at 22° C. 1 N with sodium hydroxide (1 ml) and the resulting mixture was stirred for 30 min. Then 1 N hydrochloric acid (2 ml) was added and the ethanol was evaporated under reduced pressure. The residue was dissolved in ethyl acetate, washed with brine and dried over anhydrous magnesium sulfate. Evaporation of the solvent and recrystallization of the solid residue from ethyl acetate gave 0.133 g (81% yield) of the title acid as a white crystals; mp 180–181° C. 1HNMR 400 MHz (DMSO-d6) δ (ppm): 1.55–1.6 (1H, m, CH), 2.0–2.25 (3H, m, CH2 and CH), 3.43 (2H, m, CH2), 3.44 (3H, s, NCH3), 3.75 (2H, m, CH2), 3.83 (3H, s, OCH3). Anal. Calcd for C11H15N3O6S: C, 41.64; H, 4.76; N, 13.24. Found: C, 41.84; H, 4.96; N, 12.88.

후처리

  1. customthe ethanol was evaporated under reduced pressure
  2. dissolutionThe residue was dissolved in ethyl acetate
  3. washwashed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customEvaporation of the solvent and recrystallization of the solid residue from ethyl acetate

출처 및 근거

ORD 기록
ord-ff58c5bfa79b4a06bef6e8222ea57a45
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07135467B2

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