Chloroacetic Acid → HCID 18779028, 화합물

HRID 1741445노트

반응식

HRID 1741445 반응식
[H-].[Na+].[CH3:3][C:4]1[S:8][C:7]([CH2:9][CH2:10][OH:11])=[CH:6][CH:5]=1.Cl[CH2:13][C:14]([OH:16])=[O:15]>CN(C)C=O>[CH3:3][C:4]1[S:8][C:7]([CH2:9][CH2:10][O:11][CH2:13][C:14]([OH:16])=[O:15])=[CH:6][CH:5]=1

참가 물질

5

반응물 3

HCID 300Chloroacetic AcidHCID 24758Sodium hydrideHCID 1328928919498-70-5

생성물 1

HCID 18779028HCID 18779028, 화합물수율 107.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매3회

실험 절차

Sodium hydride (0.622 g) was suspended in dry dimethylformamide (5 ml) and treated dropwise with a solution of 2-(5-methyl-2-thienyl)ethanol (1.0 g) in dry dimethylformamide (5 ml). The mixture was stirred at room temperature under nitrogen for 2 hours then a solution of chloroacetic acid (0.664 g) in dry dimethylformamide (5 ml) added. The mixture was stirred at room temperature overnight. The volatiles were removed in vacuo and the residue quenched with water and extracted with ethyl acetate. The aqueous layer was adjusted to pH 2 using dilute hydrochloric acid and then extracted with ethyl acetate. This extract was washed with water, brine then dried (MgSO4). The solvent was removed in vacuo to give a brown oil (1.51 g) which was used without further purification.

후처리

  1. stirringThe mixture was stirred at room temperature overnight
  2. customThe volatiles were removed in vacuo
  3. customthe residue quenched with water
  4. extractionextracted with ethyl acetate
  5. extractionextracted with ethyl acetate
  6. washThis extract was washed with water, brine
  7. dry with materialthen dried (MgSO4)
  8. customThe solvent was removed in vacuo

출처 및 근거

ORD 기록
ord-a38cabd90e2542f69709927a39361529
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05973167

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