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Chlorosulfonyl isocyanate → HCID 53402097, 화합물

HRID 1027996
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HRID 1027996 반응식
[F:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[CH3:11])[NH:7][CH:6]=[CH:5]2.ClS([N:16]=[C:17]=O)(=O)=O>CN(C=O)C>[F:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[CH3:11])[NH:7][CH:6]=[C:5]2[C:17]#[N:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 70918Chlorosulfonyl isocyanateHCID 247292425-fluoro-6-methyl-1H-indole

생성물 1

HCID 53402097HCID 53402097, 화합물수율 100%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Into a solution of 5-fluoro-6-methyl-1H-indole (1.9 g, 12.8 mmol) in DMF (13 mL) at −78° C. was added chlorosulfonyl isocyanate (1.33 mL, 15.3 mmol). After addition the cooling bath was removed and the mixture was allowed to warm to room temperature. The mixture was then poured into ice water, filtered and washed with water and brine. The cake was then dissolved in acetonitrile and concentrated to give 5-fluoro-6-methyl-1H-indole-3-carbonitrile (2.2 g, 100%).

후처리

  1. additionAfter addition the cooling bath
  2. customwas removed
  3. additionThe mixture was then poured into ice water
  4. filtrationfiltered
  5. washwashed with water and brine
  6. dissolutionThe cake was then dissolved in acetonitrile
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-1b2fbba23a09435187eb1e697cfbab1c
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08735414B2

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