Sodium Sulfide → 2,3-Dihydro-5,6-dimethyl-3-thioxo-4-pyridazinecarbonitrile

HRID 2173471노트

반응식

HRID 2173471 반응식
Cl[C:2]1[N:3]=[N:4][C:5]([CH3:11])=[C:6]([CH3:10])[C:7]=1[C:8]#[N:9].[S-2:12].[Na+].[Na+]>C(O)(C)(C)C.CC(O)C>[CH3:10][C:6]1[C:5]([CH3:11])=[N:4][NH:3][C:2](=[S:12])[C:7]=1[C:8]#[N:9]

참가 물질

5

반응물 2

HCID 14804Sodium SulfideHCID 3340163-Chloro-5,6-dimethylpyridazine-4-carbonitrile

생성물 1

HCID 256489772,3-Dihydro-5,6-dimethyl-3-thioxo-4-pyridazinecarbonitrile

시약·촉매·용매 2

HCID 3776Isopropanol용매HCID 6386tert-Butanol용매

실험 절차

A solution of 3-chloro-5,6-dimethylpyridazine-4-carbonitrile (100 mg, 0.60 mmol) and sodium sulfide was stirred in tert-butanol (2.0 mL) in a microwave reaction vial. The vial was sealed and irradiated at 100° C. for 10 minutes. LC/MS indicated product and no remaining starting material. The reaction solution was diluted with IPA (˜10 mL) and stirred at ambient temperature for about 15 minutes, then filtered. The solids on the filter were washed with IPA. The solute was concentrated in vacuo, and the resulting solid was dried overnight at 60° C. in a vacuum oven to give the product. LC/MS: RT=0.24 min., m/z=166 [M+H]+.

후처리

  1. customThe vial was sealed
  2. customirradiated at 100° C. for 10 minutes
  3. filtrationfiltered
  4. washThe solids on the filter were washed with IPA
  5. concentrationThe solute was concentrated in vacuo
  6. customthe resulting solid was dried overnight at 60° C. in a vacuum oven
  7. customto give the product

출처 및 근거

ORD 기록
ord-3fae2a5ebada431f88ff1cc573fdb09b
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09056875B2

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