Acetamide → 2,6-Xylyl isothiocyanate

HRID 65474

반응식

HRID 65474 반응식
[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]

참가 물질

8

반응물 5

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

생성물 1

HCID 879762,6-Xylyl isothiocyanate

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 66603805toluene N,N-dimethylacetamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-69321b9344924861a5eab92e23c20ff5
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04614798

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