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Hydrochloric Acid → 7,7-dimethyl-4,5,6,7-tetrahydro-1H-pyrazolo[4,3-c]pyridine dihydrochloride

HRID 1640246
ノート
印刷プレビュー

反応式

HRID 1640246 の反応式
FC(F)(F)C(O)=O.[CH3:8][C:9]1([CH3:25])[CH2:14][N:13](C(OC(C)(C)C)=O)[CH2:12][C:11]2[CH:22]=[N:23][NH:24][C:10]1=2.[ClH:26]>ClCCl>[ClH:26].[ClH:26].[CH3:8][C:9]1([CH3:25])[CH2:14][NH:13][CH2:12][C:11]2[CH:22]=[N:23][NH:24][C:10]1=2
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 6422Trifluoroacetic acidHCID 37818370tert-Butyl 7,7-dimethyl-6,7-dihydro-1H-pyrazolo[4,3-c]pyridine-5(4H)-carboxylate

生成物 1

HCID 667221937,7-dimethyl-4,5,6,7-tetrahydro-1H-pyrazolo[4,3-c]pyridine dihydrochloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

5 mL trifluoroacetic acid were added at 0° C. to 1.6 g (6.1 mmol) tert.butyl 7,7-dimethyl-1,4,6,7-tetrahydro-pyrazolo[4,3-c]pyridine-5-carboxylate in 15 mL dichloromethane and stirred for 2 h at RT. The reaction mixture was evaporated down. The residue was taken up in ethanol and mixed with 12 mL (15 mmol) 1.25 M ethanolic HCl and then evaporated down. The residue was triturated with ethanol and the solid was separated off by suction filtering and dried.

後処理

  1. customThe reaction mixture was evaporated down
  2. customevaporated down
  3. customThe residue was triturated with ethanol
  4. customthe solid was separated off by suction
  5. filtrationfiltering
  6. customdried

出典と根拠

ORDレコード
ord-69da4fcb3be44ad6aa6fb29632c5fea4
出典データセット
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08110575B2

反応ノート

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