Ammonia methanol → HCID 178421536、化合物

反応式

[Br:1][C:2]1[CH:3]=[CH:4][C:5]([F:19])=[C:6]([C:8]2([CH3:18])[C:14]([F:16])([F:15])[CH2:13][O:12][CH2:11][C:10](=S)[NH:9]2)[CH:7]=1.[NH3:20].CO>>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([F:19])=[C:6]([C:8]2([CH3:18])[C:14]([F:16])([F:15])[CH2:13][O:12][CH2:11][C:10](=[NH:20])[NH:9]2)[CH:7]=1

参加物

反応物 2

HCID 21705897Ammonia methanol

HCID 866502735-(5-Bromo-2-fluorophenyl)-6,6-difluoro-5-methyl-1,4-oxazepane-3-thione

生成物 1

HCID 178421536HCID 178421536、化合物

実験手順

A mixture of 5-(5-bromo-2-fluorophenyl)-6,6-difluoro-5-methyl-1,4-oxazepane-3-thione (1.0 g, 2.83 mmol) and 10% NH3/MeOH (25 mL) was stirred in a sealed tube at it for 24 h. Reaction mixture was concentrated and purified by column chromatography on silica gel with 5% MeOH, 2% NH3 in chloroform to furnish the title compound as a pale brown gum. Yield=1.1 g ( ). LCMS: RtH8=0.146 [M+H]+=337.0, 339.0,

後処理

customReaction mixture
concentrationwas concentrated
custompurified by column chromatography on silica gel with 5% MeOH, 2% NH3 in chloroform

出典と根拠

ORDレコード: ord-581fc6e17f5e4464975ae06bfe1010bc
出典データセット: uspto-grants-2012_06
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08207164B2

反応ノート

読み込み中…

参加物