Water → Methyl [2-(triphenylmethoxy)ethyl]carbamodithioate

HRID 1980369ノート

反応式

HRID 1980369 の反応式
[CH3:1][S:2][C:3](=[S:8])[NH:4][CH2:5][CH2:6][OH:7].[C:9]1([C:15](Cl)([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.O>N1C=CC=CC=1>[CH3:1][S:2][C:3](=[S:8])[NH:4][CH2:5][CH2:6][O:7][C:15]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)([C:22]1[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=1)[C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1

参加物

5

反応物 3

HCID 962WaterHCID 6456Trityl chlorideHCID 13277332Methyl (2-hydroxyethyl)carbamodithioate

生成物 1

HCID 54058214Methyl [2-(triphenylmethoxy)ethyl]carbamodithioate収率 75.5%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a solution of N-(2-hydroxyethyl)dithiocarbamic acid methyl ester (7.5 g) in pyridine (40 ml) is added triphenylmethyl chloride (15 g), and the mixture is left to stand overnight at room temperature. The reaction mixture is poured into water and extracted with ethyl acetate. The extract is washed with diluted hydrochloric acid and water, dried and concentrated to remove the solvent. The residue is crystallized from a mixture of dichloromethane and ether to give N-(2-triphenylmethoxyethyl)dithiocarbamic acid methyl ester (14.73 g).

後処理

  1. waitthe mixture is left
  2. extractionextracted with ethyl acetate
  3. washThe extract is washed with diluted hydrochloric acid and water
  4. customdried
  5. concentrationconcentrated
  6. customto remove the solvent
  7. customThe residue is crystallized from a mixture of dichloromethane and ether

出典と根拠

ORDレコード
ord-25d16449d4554ffea55143854dfd5ddc
出典データセット
uspto-grants-1985_04
特許番号
US04508909

反応ノート

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