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Dimethylcarbamoyl Chloride → HCID 20322019, 화합물

HRID 436809
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HRID 436809 반응식
[CH3:1][C:2]1[CH:10]=[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][N:4]2[N:3]=1.[Cl-].[Al+3].[Cl-].[Cl-].[K].[CH3:16][N:17]([CH3:21])[C:18](Cl)=[O:19]>>[CH3:16][N:17]([CH3:21])[C:18]([C:10]1[C:2]([CH3:1])=[N:3][N:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=12)=[O:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 6598Dimethylcarbamoyl ChlorideHCID 5462222PotassiumHCID 6451240Aluminum(III) ChlorideHCID 15620341HCID 15620341, 화합물

생성물 1

HCID 20322019HCID 20322019, 화합물수율 32.5%

실험 절차

2-Methylpyrazolo[1,5-a]pyridine (3.6g) was dissolved in N,N-dimethylcarbamoyl chloride (10.8g). Aluminum chloride (8.0g) was added to the resulting solution and the mixture was heated at 130° for 3 hr and poured into ice water. The solution was made basic with potassium hydroxied solution and extracted with chloroform. The chloroform solution was dried over sodium sulfate and concentrated. The residue was distilled to give 1.8g of the objective product, bp 149°-150° (2 mmHg). Yield 32%.

후처리

  1. temperaturethe mixture was heated at 130° for 3 hr
  2. extractionextracted with chloroform
  3. dry with materialThe chloroform solution was dried over sodium sulfate
  4. concentrationconcentrated
  5. distillationThe residue was distilled

출처 및 근거

ORD 기록
ord-cad65eb8822a47a5be5ea0cc45517867
출처 데이터셋
uspto-grants-1977_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04028370

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