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Hydrochloric Acid → HCID 57228075, 화합물

HRID 1492925
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HRID 1492925 반응식
[CH3:1][C:2]1[CH:15]=[CH:14][C:5]2[S:6][CH:7]=[C:8]([CH2:9][C:10]([O:12][CH3:13])=[O:11])[C:4]=2[CH:3]=1.[H-].[Na+].Cl.CN(C)[CH:21]=[O:22]>C(OC)=O>[CH3:1][C:2]1[CH:15]=[CH:14][C:5]2[S:6][CH:7]=[C:8]([C:9](=[CH:21][OH:22])[C:10]([O:12][CH3:13])=[O:11])[C:4]=2[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 6228Dimethylformamide2회HCID 24758Sodium hydrideHCID 2824092Benzo[b]thiophene-3-acetic acid, 5-methyl-, methyl ester

생성물 1

HCID 57228075HCID 57228075, 화합물

시약·촉매·용매 1

HCID 7865Methyl formate용매

실험 절차

A solution of 79.7 g of methyl 5-methyl-3-benzo[b]thienylacetate in 200 ml of dimethylformamide and 200 ml of methyl formate is slowly added dropwise to a suspension of 10.4 g of sodium hydride in 100 ml of dimethylformamide. The reaction mixture is stirred for 2 hours at room temperature and then acidified with dilute hydrochloric acid, and this is then extracted with ethyl acetate. The organic phase is washed with water, dried over anhydrous sodium sulfate and concentrated under reduced pressure. In this manner, methyl α-(5-methyl-3-benzo[b]thienyl)-β-hydroxyacrylate is obtained as the crude product which is used unpurified as the starting material in the next process step.

후처리

  1. extractionthis is then extracted with ethyl acetate
  2. washThe organic phase is washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-aba1dad1acfc4343b46d865e4eafaa03
출처 데이터셋
uspto-grants-1994_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05376677

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