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Acetic-formic anhydride → Ethyl [(5,7-difluoro-1,2,3,4-tetrahydronaphthalen-2-yl)(formyl)amino]acetate

HRID 863079
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HRID 863079 반응식
[CH2:1]([O:3][C:4](=[O:19])[CH2:5][NH:6][CH:7]1[CH2:16][CH2:15][C:14]2[C:9](=[CH:10][C:11]([F:18])=[CH:12][C:13]=2[F:17])[CH2:8]1)[CH3:2].[CH:20](OC(=O)C)=[O:21]>C(Cl)Cl>[CH2:1]([O:3][C:4](=[O:19])[CH2:5][N:6]([CH:7]1[CH2:16][CH2:15][C:14]2[C:9](=[CH:10][C:11]([F:18])=[CH:12][C:13]=2[F:17])[CH2:8]1)[CH:20]=[O:21])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 75269Acetic-formic anhydrideHCID 19699373Ethyl [(5,7-difluoro-1,2,3,4-tetrahydronaphthalen-2-yl)amino]acetate

생성물 1

HCID 19699354Ethyl [(5,7-difluoro-1,2,3,4-tetrahydronaphthalen-2-yl)(formyl)amino]acetate수율 97.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

A solution of ethyl[(5,7-difluoro-1,2,3,4-tetrahydronaphthalen-2-yl)-amino]acetate (7.15 g, 25.6 mmol) in 20 mL of methylene chloride under argon was cooled to approximately 0° C. Acetic formic anhydride (9.7 mL, 67.3 mmol) was cooled to 0° C. and added over 5 to 10 minutes. The mixture was stirred 0° C. for 2 hours and then allowed to warm to room temperature. The solvent was removed by co-evaporation with toluene (3×50 mL). Crystallization of the residue under high vacuum gave ethyl[(5,7-difluoro-1,2,3,4-tetrahydronaphthalen-2-yl)(formyl)amino]acetate (7.68 g, 25.0 mmol).

후처리

  1. additionadded over 5 to 10 minutes
  2. temperatureto warm to room temperature
  3. customThe solvent was removed by co-evaporation with toluene (3×50 mL)
  4. customCrystallization of the residue under high vacuum

출처 및 근거

ORD 기록
ord-4cfba093383943c5b0af534e2025c100
출처 데이터셋
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05719280

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