Hydroxyamine hydrochloride → N-({6-[(hydroxyimino)methyl]pyridin-2-yl}methoxy)-1-(1-methyl-1H-tetrazol-5-yl)-1-phenylmethanimine

HRID 1258585

反応式

HRID 1258585 の反応式
[CH3:1][N:2]1[C:6]([C:7](=[N:14][O:15][CH2:16][C:17]2[N:22]=[C:21]([CH:23]=O)[CH:20]=[CH:19][CH:18]=2)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[N:5][N:4]=[N:3]1.Cl.[NH2:26][OH:27]>N1C=CC=CC=1>[OH:27][N:26]=[CH:23][C:21]1[N:22]=[C:17]([CH2:16][O:15][N:14]=[C:7]([C:6]2[N:2]([CH3:1])[N:3]=[N:4][N:5]=2)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:18]=[CH:19][CH:20]=1

参加物

4

反応物 2

HCID 443297Hydroxyamine hydrochlorideHCID 866531376-[({[(1-methyl-1H-tetrazol-5-yl)(phenyl)methylene]amino}oxy)methyl]pyridine-2-carbaldehyde

生成物 1

HCID 136352703N-({6-[(hydroxyimino)methyl]pyridin-2-yl}methoxy)-1-(1-methyl-1H-tetrazol-5-yl)-1-phenylmethanimine収率 88.2%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a solution of 6-[({[(1-methyl-1H-tetrazol-5-yl)(phenyl)methylene]amino}oxy)methyl]pyridine-2-carbaldehyde (1.8 g, 5.58 mmol, 1 eq.) in 10 ml of pyridine was added hydroxylamine hydrochloride 0.427 g, 6.14 mmol, 1.1 eq.). The reaction was stirred for 6 hrs and stood overnight. The pyridine was evaporated, and the residue was partitioned between EtOAc and water. The organic layer was separated, dried over MgSO4 and concentrated to give N-({6-[(hydroxyimino)methyl]pyridin-2-yl}methoxy)-1-(1-methyl-1H-tetrazol-5-yl)-1-phenylmethanimine (1.66 g, 88% yield) as a pale brown solid.

後処理

  1. waitstood overnight
  2. customThe pyridine was evaporated
  3. customthe residue was partitioned between EtOAc and water
  4. customThe organic layer was separated
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-27d74db051264592b77bb9d7821c0f5e
出典データセット
uspto-grants-2013_06
特許番号
US08466176B2

関連ノート

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