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Hydrochloric Acid → HCID 178434607, 화합물

HRID 1909057
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HRID 1909057 반응식
CN(C)S([N:6]1[C:10]([CH2:11][CH2:12][CH2:13][Cl:14])=[C:9]([Br:15])[C:8]([CH3:16])=[N:7]1)(=O)=O.Cl>CO>[Br:15][C:9]1[C:8]([CH3:16])=[N:7][NH:6][C:10]=1[CH2:11][CH2:12][CH2:13][Cl:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 665996314-Bromo-5-(3-chloro-propyl)-3-methyl-pyrazole-1-sulfonic acid dimethylamide

생성물 1

HCID 178434607HCID 178434607, 화합물수율 91.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 4-bromo-5-(3-chloro-propyl)-3-methyl-pyrazole-1-sulfonic acid dimethylamide (3.85 g, 11.2 mmol) in MeOH (50 ml) at 0° C. was added 6 N HCl (50 mL). The reaction was warmed to room temperature and stirred overnight. The reaction was quenched by adding concentrated NH4OH until a pH of 8 was obtained. After concentrating to remove the MeOH, the remaining reaction solution was extracted with EtOAc and the organic layer was dried over Na2SO4, filtered and concentrated. The crude product was purified over normal phase silica starting with 10% EtOAc in heptane for 5 m and then increasing to 100% EtOAc over 40 m to give the desired product as a clear oil (2.42 g, 10.2 mmol). MS m/z 239.3 (M+H)+.

후처리

  1. customThe reaction was quenched
  2. additionby adding concentrated NH4OH until a pH of 8
  3. customwas obtained
  4. concentrationAfter concentrating
  5. customto remove the MeOH
  6. customthe remaining reaction solution
  7. extractionwas extracted with EtOAc
  8. dry with materialthe organic layer was dried over Na2SO4
  9. filtrationfiltered
  10. concentrationconcentrated
  11. customThe crude product was purified over normal phase silica starting with 10% EtOAc in heptane for 5 m
  12. temperatureincreasing to 100% EtOAc over 40 m

출처 및 근거

ORD 기록
ord-1bb0fc5b2d364c1688f48bae1f13d60a
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08598217B2

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