Acetamide → 2,6-Xylyl isothiocyanate

HRID 65474

反応式

HRID 65474 の反応式
[C:1]([NH2:4])(=O)[CH3:2].[H-].[Na+].[H][H].[C:9](=[S:11])=S.[CH3:12]N(C)C(=O)C.[CH:18]1[CH:23]=[CH:22]C=[CH:20][CH:19]=1>CN(C)C(=O)C.C1(C)C=CC=CC=1.O1CCCC1>[CH3:12][C:2]1[CH:20]=[CH:19][CH:18]=[C:23]([CH3:22])[C:1]=1[N:4]=[C:9]=[S:11]

参加物

8

反応物 5

HCID 178AcetamideHCID 6348Carbon DisulfideHCID 24758Sodium hydrideHCID 21705219N,N-Dimethylacetamide--benzene (1/1)HCID 178418361HCID 178418361、化合物

生成物 1

HCID 879762,6-Xylyl isothiocyanate

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 66603805toluene N,N-dimethylacetamide溶媒

実験手順

Briefly, this preparation involves first adding the acetamide to a suspension of sodium hydride in an organic solvent, preferably a N,N-dimethylacetamide/benzene solvent system. The cessation of hydrogen indicates completion of the reaction after which the reaction mixture is cooled and carbon disulfide added slowly. When tetrahydrofuran is the solvent employed, a reaction time of approximately 1.5 hours is required to provide yields in excess of 80 percent while when a mixture of N,N-dimethylacetamide/toluene is used, yields in excess of 80 percent are obtained in approximately 20 minutes.

後処理

  1. customcompletion of the reaction after which the reaction mixture
  2. temperatureis cooled
  3. customa reaction time of approximately 1.5 hours
  4. customto provide
  5. customyields in excess of 80 percent while when
  6. customyields in excess of 80 percent
  7. customare obtained in approximately 20 minutes

出典と根拠

ORDレコード
ord-69321b9344924861a5eab92e23c20ff5
出典データセット
uspto-grants-1986_09
特許番号
US04614798

関連ノート

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