Ethanol → HCID 54125531、化合物

HRID 867612ノート

反応式

HRID 867612 の反応式
[CH2:1]([N:3]([CH2:9][CH3:10])[C:4](=O)[C@H:5](Cl)[CH3:6])[CH3:2].[K].[S:12]1C=CC=C1CC(O)=O.[CH2:21]([OH:23])[CH3:22]>ClCCl>[CH2:1]([N:3]([CH2:9][CH3:10])[C:4](=[S:12])[C@H:5]([C:21](=[O:23])[CH3:22])[CH3:6])[CH3:2]

参加物

6

反応物 4

HCID 702Ethanol2 回HCID 159702-Thiopheneacetic acidHCID 5462222PotassiumHCID 13318792HCID 13318792、化合物

生成物 1

HCID 54125531HCID 54125531、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
55 °C

実験手順

(R)-N,N-Diethyl-2-chloropropionamide (20 g) dissolved in ethanol (30 cc) is added to a suspension of the potassium salt of thiolacetic acid (16 g) in ethanol (70 cc). The reaction mixture is then heated for 2 hours at a temperature in the vicinity of 55° C. and then concentrated to dryness under reduced pressure (130 Pa) at a temperature in the vicinity of 60° C. The residue obtained is crushed in dichloromethane (300 cc) and then washed with distilled water (200 cc). The organic phase is decanted, dried over sodium sulphate, filtered and then concentrated to dryness under reduced pressure (2.7 kPa) at a temperature in the vicinity of 30° C. The residue obtained is distilled under reduced pressure (17 Pa). (S)-N,N-Diethyl-2-acetylthiopropionamide (22 g) in the form of a slightly yellow oil [b.p.17Pa =105°-107° C.; [α]D20 =-169° (c=10; CHCl3)] is thereby obtained.

後処理

  1. concentrationconcentrated to dryness under reduced pressure (130 Pa) at a temperature in the vicinity of 60° C
  2. customThe residue obtained
  3. washwashed with distilled water (200 cc)
  4. customThe organic phase is decanted
  5. dry with materialdried over sodium sulphate
  6. filtrationfiltered
  7. concentrationconcentrated to dryness under reduced pressure (2.7 kPa) at a temperature in the vicinity of 30° C
  8. customThe residue obtained
  9. distillationis distilled under reduced pressure (17 Pa)

出典と根拠

ORDレコード
ord-d6f4a217e393461d9704f20f82ab1373
出典データセット
uspto-grants-1988_10
特許番号
US04775753

反応ノート

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