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Ammonium Hydroxide → HCID 68444152, 화합물

HRID 388954
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HRID 388954 반응식
Cl[C:2]1[CH:19]=[C:18](F)[C:17]([N+:21]([O-:23])=[O:22])=[CH:16][C:3]=1[C:4]([NH:6][C:7]1[CH:15]=[C:14]2[C:10]([CH:11]=[N:12][NH:13]2)=[CH:9][CH:8]=1)=[O:5].[NH4+].[OH-].[NH2:26]C1C=C(F)C([N+]([O-])=O)=CC=1C(NC1C=C2C(C=NN2)=CC=1)=O.[CH3:49][CH:50]1[CH2:55][NH:54][CH2:53][CH:52]([CH3:56])[NH:51]1>O1CCOCC1>[NH2:26][C:18]1[C:17]([N+:21]([O-:23])=[O:22])=[CH:16][C:3]([C:4]([NH:6][C:7]2[CH:15]=[C:14]3[C:10]([CH:11]=[N:12][NH:13]3)=[CH:9][CH:8]=2)=[O:5])=[C:2]([N:54]2[CH2:53][CH:52]([CH3:56])[NH:51][CH:50]([CH3:49])[CH2:55]2)[CH:19]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 14923Ammonium HydroxideHCID 660562,6-DimethylpiperazineHCID 68443954HCID 68443954, 화합물HCID 68446177HCID 68446177, 화합물

생성물 1

HCID 68444152HCID 68444152, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A solution of 2-chloro-4-fluoro-N-(1H-indazol-6-yl)-5-nitrobenzamide (1 mmol) in dioxane (2 mL) was reacted with aqueous NH4OH using the conditions described in Example 115. After the formation of 2-amino-4-fluoro-N-(1H-indazol-6-yl)-5-nitrobenzamide was complete, the reaction mixture was charged with 2,6-dimethylpiperazine (6 mmol). The contents were heated at reflux for 10 h, and the reaction mixture was cooled to RT. The contents were poured onto ice cold water with vigorous stirring. The solid formed was collected by filtration, washed with water, and dried in vacuo to provide the product, 4-amino-2-(3,5-dimethyl-piperazin-1-yl)-N-(1H-indazol-6-yl)-5-nitrobenzamide as a yellow solid.

후처리

  1. temperatureThe contents were heated
  2. temperatureat reflux for 10 h
  3. additionThe contents were poured onto ice cold water with vigorous stirring
  4. customThe solid formed
  5. filtrationwas collected by filtration
  6. washwashed with water
  7. customdried in vacuo

출처 및 근거

ORD 기록
ord-f3002b9760fe4eeea15f6c5c3d51cbbd
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08377983B2

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