2-Mercaptoethanol → HCID 178472918, 화합물

HRID 1834796노트

반응식

HRID 1834796 반응식
Cl[CH2:2][C:3](=[O:12])[C:4](=[N:10][OH:11])[C:5]([O:7][CH2:8][CH3:9])=[O:6].[SH:13][CH2:14][CH2:15][OH:16].C(N(CC)CC)C>C(Cl)(Cl)Cl>[OH:16][CH2:15][CH2:14][S:13][CH2:2][C:3](=[O:12])[C:4](=[N:10][OH:11])[C:5]([O:7][CH2:8][CH3:9])=[O:6]

참가 물질

5

반응물 3

HCID 15672-MercaptoethanolHCID 8471TriethylamineHCID 178472915HCID 178472915, 화합물

생성물 1

HCID 178472918HCID 178472918, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매2회

반응 조건

온도
20 °C

실험 절차

Ethyl 4-chloro-2-hydroxyimino-3-oxo-butyrate (340 g.) is dissolved in chloroform (1.5 liters) and 2-mercapto-ethanol (126 cc.) is then added. Triethylamine (248 cc.) dissolved in chloroform (1 liter) is added to the resulting solution at about 20° C., over the course of 30 minutes. The reagents are left in contact for 15 hours whilst stirring at about 20° C. Then the reaction mixture is washed with water (200 cc.) followed by 2 N hydrochloric acid (200 cc.) and finally four times with water (a total of 1 liter). The organic phase is dried over sodium sulphate treated with decolourising charcoal, filtered and concentrated to dryness under reduced pressure (20 mm.Hg). Ethyl 4-(2-hydroxy-ethylthio)-2-hydroxyimino-3-oxo-butyrate (321 g.) is thus obtained in the form of an oil which gradually solidifies.

후처리

  1. additionis added to the resulting solution at about 20° C., over the course of 30 minutes
  2. washThen the reaction mixture is washed with water (200 cc.)
  3. dry with materialThe organic phase is dried over sodium sulphate
  4. additiontreated with decolourising charcoal
  5. filtrationfiltered
  6. concentrationconcentrated to dryness under reduced pressure (20 mm.Hg)

출처 및 근거

ORD 기록
ord-176d1402f0934ddd8a5419367dc68c22
출처 데이터셋
uspto-grants-1978_01
특허 번호
US04071531

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