Thionyl Chloride → HCID 11694729、化合物

反応式

S(Cl)([Cl:3])=O.[CH3:5][O:6][C:7]1[CH:8]=[C:9]([C:13]2[O:14][C:15]([CH3:20])=[C:16]([CH3:19])[N+:17]=2[O-])[CH:10]=[CH:11][CH:12]=1>>[ClH:3].[Cl:3][CH2:19][C:16]1[N:17]=[C:13]([C:9]2[CH:10]=[CH:11][CH:12]=[C:7]([O:6][CH3:5])[CH:8]=2)[O:14][C:15]=1[CH3:20]

参加物

反応物 2

HCID 24386Thionyl Chloride

HCID 57718887HCID 57718887、化合物

生成物 1

HCID 11694729HCID 11694729、化合物

実験手順

The entire toluenic solution from Example 1 (420 ml) was admixed at 60° C. dropwise with 54.2 g (0.456 mol) of thionyl chloride and stirred at <60° C. for up to 22 h. Subsequently, the mixture was concentrated by distilling off 229 ml. The suspension was cooled to <20° C., and the product was isolated by filtration with suction, washed 3 times with 20 ml each time of toluene and dried at elevated temperature under reduced pressure.

後処理

concentrationSubsequently, the mixture was concentrated
distillationby distilling off 229 ml
temperatureThe suspension was cooled to <20° C.
customthe product was isolated by filtration with suction
washwashed 3 times with 20 ml each time of toluene
customdried at elevated temperature under reduced pressure

出典と根拠

ORDレコード: ord-d876d6e31643418faa6c38ee35b139b5
出典データセット: uspto-grants-2009_06
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US07544809B2

反応ノート

読み込み中…

参加物