Water → HCID 66855418, 화합물

HRID 2282120노트

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HRID 2282120 반응식
[C:1]([C:3]1[C:4]([C:14]2[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][C:15]=2[Cl:21])=[C:5]([C:9]([O:11]CC)=[O:10])[S:6][C:7]=1[I:8])#[N:2].O1CCCC1.O.[OH-].[Na+]>Cl>[C:1]([C:3]1[C:4]([C:14]2[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][C:15]=2[Cl:21])=[C:5]([C:9]([OH:11])=[O:10])[S:6][C:7]=1[I:8])#[N:2]

참가 물질

6

반응물 4

HCID 962WaterHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 59250036HCID 59250036, 화합물

생성물 1

HCID 66855418HCID 66855418, 화합물수율 99%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

To a solution of ethyl 4-cyano-3-(2,4-dichlorophenyl)-5-iodothiophene-2-carboxylate (1.26 g, 0.00279 mol) in Tetrahydrofuran (20 mL, 0.3 mol) was added water (9.2 mL, 0.51 mol) and 1M NaOH (19.5 mL, 0.0195 mol) and the solution was stirred at room temperature for 2 days. The mixture was acidified by 1M HCl (20 mL), extracted with EtOAc (3×100 mL). The organic extracts were combined, dried over Na2SO4, filtered and evaporated to afford the product (1.17 g, 99%). LCMS: (FA) ES+, 424, 426. 1H NMR (400 MHz, d1-chloroform) δ: 7.62-7.60 (m, 1H) 7.45-7.41 (m, 1H), 7.36-7.33 (m, 1H).

후처리

  1. extractionextracted with EtOAc (3×100 mL)
  2. dry with materialdried over Na2SO4
  3. filtrationfiltered
  4. customevaporated

출처 및 근거

ORD 기록
ord-2c22270233a8437981fdf3724af3be51
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09139589B2

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