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Water → 4-iodo-1H-indazol-3-amine

HRID 497602
ノート
印刷プレビュー

反応式

HRID 497602 の反応式
O.[NH2:2][NH2:3].F[C:5]1[CH:12]=[CH:11][CH:10]=[C:9]([I:13])[C:6]=1[C:7]#[N:8].O>C(O)C>[I:13][C:9]1[CH:10]=[CH:11][CH:12]=[C:5]2[C:6]=1[C:7]([NH2:8])=[N:2][NH:3]2
参加物反応条件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 962WaterHCID 24654Hydrazine hydrate (1:1)HCID 5227222-Fluoro-6-iodobenzonitrile

生成物 1

HCID 40577874-iodo-1H-indazol-3-amine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
78 °C

実験手順

1.2 cm3 of hydrazine monohydrate are added to 2 g of 2-fluoro-6-iodobenzonitrile in 25 cm3 of ethanol. The reaction medium is then refluxed at about 78° C. for 12 hours. The medium is allowed to return to about 20° C. and 20 cm 3 of distilled water are then added in order to precipitate the product. The insoluble material is filtered on a sinter funnel, rinsed with 20 cm3 of distilled water and then taken up in 20 cm3 of dichloromethane. The organic phase is then dried over magnesium sulphate and evaporated under reduced pressure (2 kPa; 45° C.). After drying (90 Pa; 50° C.), 1.65 g of 4-iodo-1H-indazole-3-amine are obtained in the form of a yellow solid melting at 157° C.

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート

後処理

  1. customto return to about 20° C.
  2. customto precipitate the product
  3. filtrationThe insoluble material is filtered on a sinter funnel
  4. washrinsed with 20 cm3 of distilled water
  5. dry with materialThe organic phase is then dried over magnesium sulphate
  6. customevaporated under reduced pressure (2 kPa; 45° C.)
  7. dry with materialAfter drying (90 Pa; 50° C.), 1.65 g of 4-iodo-1H-indazole-3-amine

出典と根拠

ORDレコード
ord-2ae53273fb014e0881c0daf7302f8d3a
出典データセット
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06949579B2

反応ノート

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