Ethyl trifluoroacetate → HCID 178517786, 화합물

HRID 351400노트

반응식

HRID 351400 반응식
[NH2:1][C:2]1[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][C:3]=1[C:4]([NH2:6])=[O:5].[F:12][C:13]([F:20])([F:19])[C:14](OCC)=O.[O-]CC.[Na+].CC(O)=O.O>C(O)C>[Cl:11][C:8]1[CH:7]=[C:3]2[C:2](=[CH:10][CH:9]=1)[N:1]=[C:14]([C:13]([F:20])([F:19])[F:12])[N:6]=[C:4]2[OH:5]

참가 물질

6

반응물 4

HCID 9794Ethyl trifluoroacetateHCID 788762-Amino-5-chlorobenzamideHCID 2723922Sodium ethoxideHCID 21899381Acetic acid--water (1/1)

생성물 1

HCID 178517786HCID 178517786, 화합물수율 92.7%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

2-Amino-5-chlorobenzamide (Avocado)(1.00 g, 5.86 mmol, 1.0 eq.) and ethyl trifluoroacetate (4.19 mL, 35.2 mmol, 6.0 eq.) were dissolved in 50 mL of ethanol at rt under nitrogen and followed by the addition of 3.09 M sodium ethoxide in ethanol (11.38 mL, 35.2 mmol, 6.0 eq.) The mixture was refluxed 20 hours. Cooled to rt. Added 10 mL of 10% HOAc/H2O. Solids formed which were filtered, rinsed with 5 mL H2O, then dissolved in 20 mL of EtOAc/THF. Dried and stripped in vacuo to give 1.35 g of amber solids. LCMS detects (M+H)+=249.

후처리

  1. temperaturewas refluxed 20 hours
  2. customSolids formed which
  3. filtrationwere filtered
  4. washrinsed with 5 mL H2O
  5. dissolutiondissolved in 20 mL of EtOAc/THF
  6. customDried

출처 및 근거

ORD 기록
ord-aca0adabeade49c2af4bc0682854cb96
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07183270B2

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