Hydrochloric Acid → HCID 15020141、化合物

HRID 1898782ノート

反応式

HRID 1898782 の反応式
[OH-].[Na+].[C:3]([O:18]CC)(=[O:17])[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][S:11][CH2:12][CH2:13][O:14][CH2:15][CH3:16].Cl>CO>[C:3]([OH:18])(=[O:17])[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][S:11][CH2:12][CH2:13][O:14][CH2:15][CH3:16]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 15020144HCID 15020144、化合物

生成物 1

HCID 15020141HCID 15020141、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

NaOH (1M, 24 mL, 24 mmol) was added to a solution of the above ethyl 9-thia-12-oxatetradecanoate. (6.8 mmol) in MeOH (20 mL). After stirring for 7 h, the reaction mixture was acidified with 10% HCl (pH 1) and extracted with ethyl acetate (2×100 mL). The organic phase was washed with water (50 mL), brine (50 mL), and dried (Na2SO4). The crude product was recrystallized from hexane to afford the title compound, 9-thia-12-oxatetradecanoic acid; yield 92%; bp 134°-136° C./0.005 torr; IR (neat): 3000 (broad) and 1735 cm-1NMR: 1.23 (3H, t, J=7.2 Hz), 1.28-1.46 (6H, m), 1.53-1.68 (4H, m), 2.35 (2H, t, J=7.3 Hz), 2.54 (2H, t, J=7.1 Hz), 2.70 (2H, t, J=7.1 Hz), 3.52 (2H, q, J=7.2 Hz), 3.60 (2H, t, J=6.9 Hz), and 8.85 ppm (1H, br s); Found: C, 57.96, H, 9.77%. Calcd for C12H24SO3 : C, 58.03, H, 9.74%.

後処理

  1. extractionextracted with ethyl acetate (2×100 mL)
  2. washThe organic phase was washed with water (50 mL), brine (50 mL)
  3. dry with materialdried (Na2SO4)
  4. customThe crude product was recrystallized from hexane

出典と根拠

ORDレコード
ord-d6d4679542854f5faefb0019b4f58361
出典データセット
uspto-grants-1996_11
特許番号
US05571689

反応ノート

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