Ethanol → HCID 54125531, 화합물

HRID 867612노트

반응식

HRID 867612 반응식
[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]

참가 물질

6

반응물 4

HCID 702Ethanol2회HCID 159702-Thiopheneacetic acidHCID 5462222PotassiumHCID 13318792HCID 13318792, 화합물

생성물 1

HCID 54125531HCID 54125531, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
55 °C

실험 절차

(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.

후처리

  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)

출처 및 근거

ORD 기록
ord-d6f4a217e393461d9704f20f82ab1373
출처 데이터셋
uspto-grants-1988_10
특허 번호
US04775753

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