Sodium Carbonate → HCID 178472137, 화합물

HRID 1168529

반응식

HRID 1168529 반응식
[CH:1]([N:3]([CH3:5])[NH2:4])=[O:2].[F:6][C:7]1[C:24]([F:25])=[CH:23][C:22]([I:26])=[CH:21][C:8]=1[C:9]([C:11](=[CH:17]OCC)[C:12]([O:14][CH2:15][CH3:16])=[O:13])=[O:10].C([O-])([O-])=O.[Na+].[Na+]>C1(C)C=CC=CC=1>[F:6][C:7]1[C:24]([F:25])=[CH:23][C:22]([I:26])=[CH:21][C:8]=1[C:9]([C:11](=[CH:17][NH:4][N:3]([CH:1]=[O:2])[CH3:5])[C:12]([O:14][CH2:15][CH3:16])=[O:13])=[O:10]

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 12962Hydrazinecarboxaldehyde, 1-methyl-HCID 69879816Ethyl 2-(2,3-Difluoro-5-iodobenzoyl)-3-ethoxy-2-propenoate

생성물 1

HCID 178472137HCID 178472137, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매3회

실험 절차

A solution of 1-formyl-1-methylhydrazine (0.217 g) in toluene (0.5 mL) is added to a solution of ethyl 2-(2,3-difluoro-5-iodobenzoyl)-3-ethoxy-2-propenoate (Preparation 21, 1.00 g) in toluene (2.5 mL) at 33° C. After stirring at ambient temperature for 20 minutes, a precipitate formed and an additional 1.5 mL of toluene is added. After an additional 1.75 h, solid anhydrous Na2CO3 (0.285 g) is added and the reaction mixture is heated to reflux. After 1 h, the reaction mixture is concentrated at reduced pressure and the residue suspended in 8 mL of water which is used as is in the following step. Physical characteristics: MS (ESI+) m/z 419 (M+H)+.

후처리

  1. customa precipitate formed
  2. waitAfter an additional 1.75 h
  3. temperaturethe reaction mixture is heated to reflux
  4. waitAfter 1 h
  5. concentrationthe reaction mixture is concentrated at reduced pressure

출처 및 근거

ORD 기록
ord-9e8961366057427c8c487a5a6fc100ca
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06624159B2

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