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Hydrochloric Acid → HCID 178434607、化合物

HRID 1909057
ノート
印刷プレビュー

反応式

HRID 1909057 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 178434607HCID 178434607、化合物収率 91.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-1bb0fc5b2d364c1688f48bae1f13d60a
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08598217B2

反応ノート

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