Water → HCID 178512066、化合物

HRID 2242886

反応式

HRID 2242886 の反応式
[Br:1][C:2]1[C:3]([NH2:9])=[N:4][CH:5]=[C:6]([Br:8])[N:7]=1.[O:10]1[CH:14]=[CH:13][CH:12]=[C:11]1[C:15]#[N:16].[Al+3].[Cl-].[Cl-].[Cl-].O>ClC(Cl)C>[Br:1][C:2]1[C:3]([NH:9][C:15]([C:11]2[O:10][CH:14]=[CH:13][CH:12]=2)=[NH:16])=[N:4][CH:5]=[C:6]([Br:8])[N:7]=1

参加物

6

反応物 4

HCID 962WaterHCID 692452-FuronitrileHCID 6200042-Amino-3,5-dibromopyrazineHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 178512066HCID 178512066、化合物収率 72%

試薬・触媒・溶媒 1

HCID 63651,1-Dichloroethane溶媒

実験手順

A solution of 3,5-dibromo-pyrazin-2-ylamine (608 mg, 2.4 mmol), furan-2-carbonitrile (297 uL, 3.39 mmol) and AlCl3 (320 mg, 2.4 mmol) in dichloroethane (6 ml) was heated at 115° C. overnight. The reaction was cooled to room temperature and water (5 ml) was added. After 30 minutes, the resulting precipitate was collected and purified by column chromatography (SiO2, THF) to afford 595 mg (72%) of N-(3,5-dibromo-pyrazin-2-yl)-furan-2-carboxamidine as a yellow solid. 1H NMR (300 MHz, DMSO-d6) δ 6.73 (dd, J=3.4, 1.8 Hz, 1H), 7.3 (dd, J=3.1 Hz, 1H), 7.98 (s, 1H), 8.49(s, 1H), 8.69 (br. s, 1H).

後処理

  1. customthe resulting precipitate was collected
  2. custompurified by column chromatography (SiO2, THF)

出典と根拠

ORDレコード
ord-e652283c74b74d7c9aa07581e79364ed
出典データセット
uspto-grants-2010_03
特許番号
US07674791B2

関連ノート

読み込み中…