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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 86721240、化合物

HRID 1750396
ノート
印刷プレビュー

反応式

HRID 1750396 の反応式
[Br:1][C:2]1[N:6]([C:7]([CH3:10])([CH3:9])[CH3:8])[N:5]=[CH:4][C:3]=1[C:11]([OH:13])=O.CC[N:16]=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1.[Cl-].[NH4+]>CN(C=O)C>[Br:1][C:2]1[N:6]([C:7]([CH3:10])([CH3:9])[CH3:8])[N:5]=[CH:4][C:3]=1[C:11]([NH2:16])=[O:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 25517Ammonium ChlorideHCID 757711-HydroxybenzotriazoleHCID 861361105-bromo-1-tert-butyl-1H-pyrazole-4-carboxylic acid

生成物 1

HCID 86721240HCID 86721240、化合物収率 60.3%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

A solution of the compound (10.29 g, 41.64 mmol) obtained in step 3, WSC (9.58 g, 49.97 mmol), HOBt (6.75 g, 49.97 mmol), TEA (6.97 ml, 49.97 mmol) and ammonium chloride (2.67 g, 49.97 mmol) in DMF (100 mL) was stirred at room temperature for 14 hr. The reaction mixture was concentrated under reduced pressure, and water and ethyl acetate were added to the residue. The organic layer was washed with water, aqueous sodium hydrogen carbonate solution and saturated brine and dried, and the solvent was evaporated under reduced pressure to give 5-bromo-1-tert-butyl-1H-pyrazole-4-carboxamide (6.18 g, 25.1 mmol, 60%) as a white powder.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure, and water and ethyl acetate
  2. additionwere added to the residue
  3. washThe organic layer was washed with water, aqueous sodium hydrogen carbonate solution and saturated brine
  4. customdried
  5. customthe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-ea380e68f08b49088017fcebde91740a
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09156837B2

反応ノート

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