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Beta-Propiolactone → 3-[(2-Methylphenyl)thio]propanoic acid

HRID 50966
ノート
印刷プレビュー

反応式

HRID 50966 の反応式
[CH3:1][C:2]1[C:7]([SH:8])=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:9]1(=[O:13])[O:12][CH2:11][CH2:10]1>C(#N)C>[CH3:1][C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][C:7]=1[S:8][CH2:11][CH2:10][C:9]([OH:13])=[O:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 2365Beta-Propiolactone2 回HCID 87122-Thiocresol

生成物 1

HCID 2685443-[(2-Methylphenyl)thio]propanoic acid収率 59%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A solution of acetonitrile (30 mL) and o-thiocresol (5.0 g, 40 mmol) was heated to reflux. Neat β-propiolactone (2.8 mL, 40 mmol) was added dropwise over 5 min. Heating was continued at reflux for 20 h at which time additional β-propiolactone (2.8 mL, 40 mmol) was added in one portion. After heating for an additional 24 h, the reaction mixture was concentrated in vacuo. The resultting solid-oil mixture was treated at 23° C. with 2N aqueous NaOH (150 mL). This basic solution was washed with Et2O (2×200 mL). The separated aqueous layer was acidified with conc. aqueous HCl until pH<1. This heterogenous solution was concentrated in vacuo to half of its original volume. Then it was allowed to stand at 23° C. for 2 h. The solid product was collected by vacuum filtration, washed with H2O (20 mL), and dried under vacuum at 65° C. for 2 h to afford 3-[(2-methylphenyl)sulfanyl]propanoic acid (4.62 g, 59%) as a white powder. 1H NMR (CHCl3, 300 MHz) δ7.31 (d, 1H, J=7.0 Hz), 7.20-7.15 (m, 3H), 3.14 (t, 2H, J=7.3 Hz), 2.69 (t, 2H, J=7.4 Hz), 2.39 (s, 3H) ppm.

後処理

  1. temperatureHeating
  2. additionwas added in one portion
  3. temperatureAfter heating for an additional 24 h
  4. concentrationthe reaction mixture was concentrated in vacuo
  5. additionThe resultting solid-oil mixture was treated at 23° C. with 2N aqueous NaOH (150 mL)
  6. washThis basic solution was washed with Et2O (2×200 mL)
  7. concentrationThis heterogenous solution was concentrated in vacuo to half of its original volume
  8. filtrationThe solid product was collected by vacuum filtration
  9. washwashed with H2O (20 mL)
  10. customdried under vacuum at 65° C. for 2 h

出典と根拠

ORDレコード
ord-dddda26eb0fe48a782d553cdeb5fd39f
出典データセット
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06713471B1

反応ノート

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