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Carbon Disulfide → HCID 11020189、化合物

HRID 1954476
ノート
印刷プレビュー

反応式

HRID 1954476 の反応式
[CH2:1]([C:3]1[CH:9]=[CH:8][C:6]([NH2:7])=[CH:5][CH:4]=1)[CH3:2].[C:10](=[S:12])=[S:11].[CH2:13](N(CC)CC)C.CCCCCC>C(OCC)C>[CH2:1]([C:3]1[CH:9]=[CH:8][C:6]([NH:7][C:10](=[S:12])[S:11][CH3:13])=[CH:5][CH:4]=1)[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6348Carbon DisulfideHCID 8058HexaneHCID 8471TriethylamineHCID 115044-Ethylaniline

生成物 1

HCID 11020189HCID 11020189、化合物収率 69.8%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

To a solution of 4-ethylaniline (7.8 g) in diethyl ether (40 ml) were added carbon disulfide (6 g) and triethylamine (13 g). After stirring at room temperature for 2 hours, the precipitated crystals were collected by filtration and dried. The crystals (16 g) were dissolved in methanol (100 ml) and methyl iodide (7.6 g) was added dropwise thereto. The mixture was stirred at room temperature for 2 hours, acidified (pH =about 2) with in HCl and extracted with ethyl acetate. The organic phase was washed with water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure to give a solid. The solid was treated with hexane, triturated, filtered and dried to give the desired methyl 4-ethylphenyldithiocarbamate (9.5 g, yield: 67%), m.p. 78° C.

後処理

  1. filtrationthe precipitated crystals were collected by filtration
  2. customdried
  3. dissolutionThe crystals (16 g) were dissolved in methanol (100 ml)
  4. additionmethyl iodide (7.6 g) was added dropwise
  5. stirringThe mixture was stirred at room temperature for 2 hours
  6. extractionextracted with ethyl acetate
  7. washThe organic phase was washed with water
  8. dry with materialdried over anhydrous magnesium sulfate
  9. concentrationconcentrated under reduced pressure
  10. customto give a solid
  11. customtriturated
  12. filtrationfiltered
  13. customdried

出典と根拠

ORDレコード
ord-125b19df9f1d43aaa9bebd49ce51a070
出典データセット
uspto-grants-2000_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06121476

反応ノート

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