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3-(Trifluoromethyl)aniline → Ethyl 3-oxo-3-{[3-(trifluoromethyl)phenyl]amino}propanoate

HRID 559785
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반응식

HRID 559785 반응식
[F:1][C:2]([F:11])([F:10])[C:3]1[CH:4]=[C:5]([CH:7]=[CH:8][CH:9]=1)[NH2:6].C(N(CC)CC)C.Cl[C:20](=[O:27])[CH2:21][C:22]([O:24][CH2:25][CH3:26])=[O:23]>CC(C)=O>[O:27]=[C:20]([NH:6][C:5]1[CH:7]=[CH:8][CH:9]=[C:3]([C:2]([F:10])([F:11])[F:1])[CH:4]=1)[CH2:21][C:22]([O:24][CH2:25][CH3:26])=[O:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 73753-(Trifluoromethyl)anilineHCID 8471TriethylamineHCID 118931Ethyl 3-chloro-3-oxopropionate

생성물 1

HCID 3651864Ethyl 3-oxo-3-{[3-(trifluoromethyl)phenyl]amino}propanoate수율 99%

시약·촉매·용매 1

HCID 180Acetone용매2회

실험 절차

To an ice-cooled solution of 3-(trifluoromethyl)aniline (64.5 g, 0.40 mol) and triethylamine (60 ml) in acetone (700 ml) was added dropwise, ethyl 3-chloro-3-oxopropanoate (63.6 g, 0.42 mol) in acetone (50 ml). After the addition (approx. 30 minutes) stirring was continued at room temperature overnight. The solvents were removed and water (1200 ml) was added. The resulting precipitate was filtered off, thoroughly washed twice with water and then dried to afford the title compound as yellow powder (109 g, 99%).

후처리

  1. additionwas added dropwise
  2. additionAfter the addition (approx. 30 minutes)
  3. customThe solvents were removed
  4. additionwater (1200 ml) was added
  5. filtrationThe resulting precipitate was filtered off
  6. washthoroughly washed twice with water
  7. customdried

출처 및 근거

ORD 기록
ord-c6fa927967324d328a84e49b75ed1b6f
출처 데이터셋
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08063073B2

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