Hydrochloric Acid → HCID 58739076、化合物

HRID 720278ノート

反応式

HRID 720278 の反応式
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

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 58739069HCID 58739069、化合物

生成物 1

HCID 58739076HCID 58739076、化合物収率 81%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ff58c5bfa79b4a06bef6e8222ea57a45
出典データセット
uspto-grants-2006_11
特許番号
US07135467B2

反応ノート

読み込み中…