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Sodium Carbonate → HCID 86743846、化合物

HRID 2073237
ノート
印刷プレビュー

反応式

HRID 2073237 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([NH:9][NH2:10])=[C:5]([N+:11]([O-:13])=[O:12])[CH:4]=1)#[N:2].C(=O)([O-])[O-].[Na+].[Na+].[Cl:20][C:21]1[CH:29]=[CH:28][C:24]([C:25](Cl)=[O:26])=[CH:23][C:22]=1[S:30](=[O:33])(=[O:32])[NH2:31]>O1CCOCC1>[C:1]([C:3]1[CH:8]=[CH:7][C:6]([N:9]([C:25](=[O:26])[C:24]2[CH:28]=[CH:29][C:21]([Cl:20])=[C:22]([S:30](=[O:32])(=[O:33])[NH2:31])[CH:23]=2)[NH2:10])=[C:5]([N+:11]([O-:13])=[O:12])[CH:4]=1)#[N:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 30179793-(Aminosulfonyl)-4-chlorobenzoyl chlorideHCID 35266544-Hydrazinyl-3-nitrobenzonitrile

生成物 1

HCID 86743846HCID 86743846、化合物収率 65%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

The process described in Example 1(B) was followed and 8.1 g of 4-cyano-2-nitrophenylhydrazine (prepared as described in: Beilst. 9 Vol. II page 289), 114 ml of dioxane, 46 ml aqueous solution of 2.4 g of crystalline sodium carbonate and 11.6 g of 4-chloro-3-sulfamoylbenzoyl chloride dissolved in 53 ml of dioxane were used as starting materials. After evaporating the reaction mixture, the residue was thoroughly mixed with water, the yellow precipitate was filtered by suction, washed with water and dried at 80° C. Thus, 3.75 g (65%) of 4-cyano-2-nitro-N-(4'-chloro-3'-sulfamoylbenzoyl)-phenylhydrazine were obtained, m.p.: 292°-295° C. (with decomposition) after recrystallization from acetic acid.

後処理

  1. customAfter evaporating the reaction mixture
  2. additionthe residue was thoroughly mixed with water
  3. filtrationthe yellow precipitate was filtered by suction
  4. washwashed with water
  5. customdried at 80° C

出典と根拠

ORDレコード
ord-678c2f7353054e2b8ba4f6274f14ea89
出典データセット
uspto-grants-1990_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04916149

反応ノート

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