Water → HCID 178418853、化合物

HRID 10517

反応式

HRID 10517 の反応式
[C:1]([O:5][C:6]([NH:8][C@H:9]1[CH2:14][CH2:13][C@H:12](OS(C)(=O)=O)[CH2:11][CH2:10]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C[Si]([N:24]=[N+:25]=[N-:26])(C)C.[F-].[Cs+].O>CN(C)C=O>[C:1]([O:5][C:6]([NH:8][C@@H:9]1[CH2:14][CH2:13][C@H:12]([N:24]=[N+:25]=[N-:26])[CH2:11][CH2:10]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]

参加物

6

反応物 4

HCID 962WaterHCID 25953Cesium fluorideHCID 78378AzidotrimethylsilaneHCID 178418975HCID 178418975、化合物

生成物 1

HCID 178418853HCID 178418853、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of Intermediate 36 (196 g) and trimethylsilyl azide (283 ml, Tokyo Kasei Kogyo) in dimethylformamide (667 ml) was added with cesium fluoride (305 g, Wako Pure Chemical Industries) with stirring and stirred at 70° C. for 4 days. The reaction mixture was cooled to room temperature and then added twice with water in a volume of 2.75 l in total. This reaction mixture was stirred with ice cooling for 2 hours, and the deposited precipitates were collected by filtration. Then, the precipitates were washed with water to obtain a roughly purified product of the title compound (142 g).

後処理

  1. stirringstirred at 70° C. for 4 days
  2. stirringThis reaction mixture was stirred with ice cooling for 2 hours
  3. customthe deposited precipitates
  4. filtrationwere collected by filtration
  5. washThen, the precipitates were washed with water

出典と根拠

ORDレコード
ord-b811f8e37f91454ca9c82dfe2654d854
出典データセット
uspto-grants-2006_08
特許番号
US07094789B2

関連ノート

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