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Sodium Carbonate → HCID 86743846, 화합물

HRID 2073237
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HRID 2073237 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

HCID 86743846HCID 86743846, 화합물수율 65%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-678c2f7353054e2b8ba4f6274f14ea89
출처 데이터셋
uspto-grants-1990_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04916149

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