Water → 2,3-Dihydro-2,2-dimethyl-7-benzofuranyl methyl(4-morpholinylthio)carbamate

HRID 435805

反応式

HRID 435805 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.[O:17]1[CH2:22][CH2:21][N:20]([S:23]Cl)[CH2:19][CH2:18]1.Cl.N1C=CC=CC=1.O>N1C=CC=CC=1>[CH3:15][N:14]([S:23][N:20]1[CH2:21][CH2:22][O:17][CH2:18][CH2:19]1)[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

6

反応物 4

HCID 962WaterHCID 2566CarbofuranHCID 10176127Pyridinium chlorideHCID 122977794-Morpholinesulfenyl chloride

生成物 1

HCID 413832,3-Dihydro-2,2-dimethyl-7-benzofuranyl methyl(4-morpholinylthio)carbamate収率 60.4%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A mixture of 6.6 g of carbofuran and 4.8 g of morpholinosulfenyl chloride in 40 ml of pyridine was allowed to stand at room temperature for about 18 hours. The mixture, which contained solid pyridine hydrochloride, was poured into water and the aqueous mixture extracted with diethyl ether. The ether extract was washed with dilute acid, then with water and with saturated sodium chloride solution and dried. Evaporation of the ether gave 6.1 g of 2,3-dihydro-2,2-dimethyl-7-benzofuranyl (methyl)(morpholinosulfenyl)carbamate, m.p. 75° -78° . Recrystallization from hexane-diethyl ether increased the melting point to 89° .

後処理

  1. extractionthe aqueous mixture extracted with diethyl ether
  2. extractionThe ether extract
  3. washwas washed
  4. additionwith dilute acid
  5. dry with materialwith water and with saturated sodium chloride solution and dried
  6. customEvaporation of the ether

出典と根拠

ORDレコード
ord-68289026b5b44592bd76e0767cbb162a
出典データセット
uspto-grants-1977_02
特許番号
US04006231

関連ノート

読み込み中…