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Water → Carbamic acid, N-(dimethylamino)thio-N-methyl-, 2,3-dihydro-2,2-dimethyl-7-benzofuranyl ester

HRID 435804
ノート
印刷プレビュー

反応式

HRID 435804 の反応式
[CH3:1][C:2]1([CH3:16])[O:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][C:8]=2[O:11][C:12]([NH:14][CH3:15])=[O:13])[CH2:3]1.[CH3:17][N:18]([CH3:21])[S:19]Cl.O>N1C=CC=CC=1>[CH3:17][N:18]([CH3:21])[S:19][N:14]([CH3:15])[C:12](=[O:13])[O:11][C:8]1[C:9]2[O:10][C:2]([CH3:16])([CH3:1])[CH2:3][C:4]=2[CH:5]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 2566Carbofuran2 回HCID 12297775(Dimethylamino)sulfenyl chloride

生成物 1

HCID 41382Carbamic acid, N-(dimethylamino)thio-N-methyl-, 2,3-dihydro-2,2-dimethyl-7-benzofuranyl ester

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A mixture of 16 g of carbofuran and 8.5 g of (dimethylamino)sulfenyl chloride in 50 ml of pyridine was allowed to stand at room temperature for about 18 hours. The mixture was poured into water, the aqueous mixture extracted with chloroform, the extracts washed with dilute hydrochloric acid, followed by water and saturated sodium chloride solution. Concentration under reduced pressure gave an oil which was found by nuclear magnetic resonance spectroscopy to contain about 20% unreacted carbofuran. This oil was subjected to column chromatography on silica gel using diethyl etherhexane (3:1) as eluting solvent to obtain 2,3-dihydro-2,2-dimethyl-7-benzofuranyl (dimethylaminosulfenyl)(methyl)carbamate

後処理

  1. extractionthe aqueous mixture extracted with chloroform
  2. washthe extracts washed with dilute hydrochloric acid
  3. concentrationConcentration under reduced pressure
  4. customgave an oil which
  5. washas eluting solvent

出典と根拠

ORDレコード
ord-a7fe143cb4264d67b770516fccc4a774
出典データセット
uspto-grants-1977_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04006231

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート