2-Chloroveratraldehyde → N-(2-chloro-3,4-dimethoxybenzylideneamino)-N'-hydroxy-N''-phenylguanidine

HRID 860181ノート

反応式

HRID 860181 の反応式
[Cl:1][C:2]1[C:9]([O:10][CH3:11])=[C:8]([O:12][CH3:13])[CH:7]=[CH:6][C:3]=1[CH:4]=O.S([C:18]1[CH:24]=[CH:23][C:21](C)=[CH:20][CH:19]=1)(O)(=O)=O.[OH:25][NH:26][C:27]([NH:29][NH:30]C1C=CC=CC=1)=[NH:28]>CO>[Cl:1][C:2]1[C:9]([O:10][CH3:11])=[C:8]([O:12][CH3:13])[CH:7]=[CH:6][C:3]=1[CH:4]=[N:30][NH:29][C:27]([NH:26][OH:25])=[N:28][C:18]1[CH:24]=[CH:23][CH:21]=[CH:20][CH:19]=1

参加物

4

反応物 2

HCID 794452-ChloroveratraldehydeHCID 178427661HCID 178427661、化合物

生成物 1

HCID 86590910N-(2-chloro-3,4-dimethoxybenzylideneamino)-N'-hydroxy-N''-phenylguanidine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

0.22 g (1.1 mmol) 2-chloro-3,4 dimethoxybenzaldehyde and 0.34 g (1 mmol) N-hydroxy-N′-phenylaminoguanidine tosylate was mixed in 7 ml methanol. The reaction mixture was refluxed for 80 min after which it was cooled down, to room temperature. The solvent was evaporated and 10 ml acetonitile was added and the solution was stirred for 1 h. The precipitate formed was filtered, washed with ether and subseqently dried. The yield of title compound 2 was 0.40 g (77%) as a crystalline solid M.p. 167–169° C.

後処理

  1. temperatureThe reaction mixture was refluxed for 80 min after which it
  2. customThe solvent was evaporated
  3. addition10 ml acetonitile was added
  4. customThe precipitate formed
  5. filtrationwas filtered
  6. washwashed with ether
  7. customsubseqently dried

出典と根拠

ORDレコード
ord-bf477626a78644a384a8cc8ca00661d9
出典データセット
uspto-grants-2006_12
特許番号
US07153881B2

反応ノート

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