Hydrazine hydrate (1:1) → HCID 178432964、化合物

HRID 1047293ノート

反応式

HRID 1047293 の反応式
O.[NH2:2][NH2:3].[Br:4][C:5]1[CH:6]=[CH:7][C:8]([C:12]#[N:13])=[N:9][C:10]=1[CH3:11]>C(O)C>[Br:4][C:5]1[CH:6]=[CH:7][C:8]([C:12](=[NH:13])[NH:2][NH2:3])=[N:9][C:10]=1[CH3:11]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 498187795-Bromo-6-methylpyridine-2-carbonitrile

生成物 1

HCID 178432964HCID 178432964、化合物収率 89%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
50 °C

実験手順

Hydrazine monohydrate (2 equiv) was added to a stirring 1.2 M suspension of 5-bromo-6-methylpicolinonitrile (1 equiv) in ethanol under nitrogen. The reaction mixture was heated at 50° C. for 24 h. The reaction was cooled to room temperature and then filtered. The collected solid was washed with cold ethanol followed by cold t-butyl methyl ether. The washed solid was dried under vacuum to provide the title compound in 89% yield, as a yellow solid. MS (ESI) m/z 228.9 [M]+, 230.9 [M+2]+.

後処理

  1. temperatureThe reaction was cooled to room temperature
  2. filtrationfiltered
  3. washThe collected solid was washed with cold ethanol
  4. customThe washed solid was dried under vacuum

出典と根拠

ORDレコード
ord-6892aeebd47b42418480e075c79c41ed
出典データセット
uspto-grants-2013_10
特許番号
US08569494B2

反応ノート

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