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Dimethylformamide → HCID 86752547、化合物

HRID 1289779
ノート
印刷プレビュー

反応式

HRID 1289779 の反応式
[NH2:1][C:2]1[N:6]=[C:5]([NH2:7])[N:4]([C:8]([NH:10][CH3:11])=[S:9])[N:3]=1.CN(C)[CH:14]=[O:15].[CH2:17](N(CC)CC)C.CC[C:26]([C:28](Cl)=[O:29])=[O:27]>O.C(Cl)(Cl)Cl>[NH2:7][C:5]1[N:4]([C:8]([NH:10][CH3:11])=[S:9])[N:3]=[C:2]([NH:1][C:26]([C:28]([O:15][CH2:14][CH3:17])=[O:29])=[O:27])[N:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6228DimethylformamideHCID 8471TriethylamineHCID 10725863HCID 10725863、化合物HCID 11007880Butanoyl chloride, 2-oxo-

生成物 1

HCID 86752547HCID 86752547、化合物収率 19%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6212
Chloroform
溶媒

実験手順

The compound (4.00 g) obtained in Example 31, dimethylformamide (80 ml) and triethylamine (3.9 ml) were cooled to 0° C. Ethyloxalyl chloride (2.7 ml) was gradually added dropwise and the mixture was stirred at 0° C.-room temperature for 2.5 hours. After the stirring, chloroform (50 ml) was added and the mixture was stirred at 0° C. for 30 minutes. The reaction mixture was poured into water and extracted with chloroform. The extract was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was distilled away under reduced pressure to give a pale-yellow liquid. This liquid was subjected to silica gel column chromatography (chloroform-methanol) and recrystallization from ethanol to give 1.22 g of white powdery crystals (yield 19%).

後処理

  1. stirringthe mixture was stirred at 0° C. for 30 minutes
  2. extractionextracted with chloroform
  3. washThe extract was washed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationThe solvent was distilled away under reduced pressure
  6. customto give a pale-yellow liquid
  7. customThis liquid was subjected to silica gel column chromatography (chloroform-methanol) and recrystallization from ethanol

出典と根拠

ORDレコード
ord-6954eba5541e4d9db465f6ba146872f2
出典データセット
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05750545

反応ノート

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