Water → HCID 54342136、化合物

HRID 1789815ノート

反応式

HRID 1789815 の反応式
[C:1]([O:5][C:6](=[O:16])[NH:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14]Br)=[CH:10][N:9]=1)([CH3:4])([CH3:3])[CH3:2].[CH3:17][C:18]1([CH3:28])[O:23][C:22](=[O:24])[CH:21]([CH2:25][CH3:26])[C:20](=[O:27])[O:19]1.C(N(CC)CC)C.O>CS(C)=O>[C:1]([O:5][C:6](=[O:16])[NH:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14][C:21]2([CH2:25][CH3:26])[C:20](=[O:27])[O:19][C:18]([CH3:17])([CH3:28])[O:23][C:22]2=[O:24])=[CH:10][N:9]=1)([CH3:4])([CH3:3])[CH3:2]

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 37577125-Ethyl-2,2-dimethyl-1,3-dioxane-4,6-dioneHCID 23030321tert-Butyl (5-(bromomethyl)pyridin-2-yl)carbamate

生成物 1

HCID 54342136HCID 54342136、化合物収率 87.3%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

(5-Bromomethyl-pyridin-2-yl)-carbamic acid tert-butyl ester (1.0 g, 3.48 mmol) was added to a solution of 2,2-dimethyl-5-ethyl-1,3-dioxane4,6-dione (600 mg, 3.48 mmol) and triethylamine (0.51 mL, 3.66 mmol) in dimethyl sulfoxide (40 mL) under nitrogen. The reaction mixture was stirred over night and water (100 mL) was added. Filtration of the precipitate gave [5-(5-ethyl-2,2-dimethyl-4,6-dioxo-[1,3]dioxan-5-ylmethyl)-pyridin-2-yl]-carbamic acid tert-butyl ester (1.15 g, 87%).

後処理

  1. filtrationFiltration of the precipitate

出典と根拠

ORDレコード
ord-436afded2b2d4ff79d62622977886f08
出典データセット
uspto-grants-2006_07
特許番号
US07071175B1

反応ノート

読み込み中…