Sodium Carbonate → HCID 178472137、化合物

HRID 1168529

反応式

HRID 1168529 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 178472137HCID 178472137、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒3 回

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-9e8961366057427c8c487a5a6fc100ca
出典データセット
uspto-grants-2003_09
特許番号
US06624159B2

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