2-Amino-1-butanol, (+)- → HCID 178456043、化合物

反応式

Cl[C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[C:5]([CH3:11])=[CH:4][N+:3]=1[O-:12].[NH2:13][C@@H:14]([CH2:17][CH3:18])[CH2:15][OH:16]>C(O)C>[OH:16][CH2:15][C@@H:14]([NH:13][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[C:5]([CH3:11])=[CH:4][N+:3]=1[O-:12])[CH2:17][CH3:18]

参加物

実験手順

2-Chloro-5-methyl-4-nitropyridine N-oxide (200 mg, 1.06 mmol, 1.0 equivalent) was dissolved in ethanol (1.5 mL). (S)-2-Aminobutanol (284 mg, 3.2 mmol, 3.0 equivalent) was then added and the resulting mixture was refluxed for 16 hours. The crude solution was then purified by reversed phase HPLC (acetonitrile/water/TFA) to afford the title compound as a brown solid (146 mg, 0.61 mmol, Rt(min) 3.787; FIA ES+ 241.8, ES− not observed).

後処理

temperaturethe resulting mixture was refluxed for 16 hours
customThe crude solution was then purified by reversed phase HPLC (acetonitrile/water/TFA)

出典と根拠

ORDレコード: ord-9885a9374170465580a493429f8fbffd
出典データセット: uspto-grants-2008_04
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US07354939B2

反応ノート

読み込み中…

参加物

反応物 2

HCID 1200842-Amino-1-butanol, (+)-

HCID 123180102-Chloro-5-methyl-4-nitropyridine N-oxide

生成物 1

HCID 178456043HCID 178456043、化合物収率 57.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

後処理

temperaturethe resulting mixture was refluxed for 16 hours
customThe crude solution was then purified by reversed phase HPLC (acetonitrile/water/TFA)

出典と根拠

ORDレコード: ord-9885a9374170465580a493429f8fbffd
出典データセット: uspto-grants-2008_04
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US07354939B2

反応ノート

読み込み中…