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Hydrochloric Acid → Hydrochloric Acid

HRID 511101
ノート
印刷プレビュー

反応式

HRID 511101 の反応式
C(OC([N:8]1[CH2:13][CH2:12][CH:11]([NH:14][C:15]2[CH:20]=[CH:19][C:18]([C:21]([F:24])([F:23])[F:22])=[CH:17][N:16]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O.[ClH:32]>ClCCl.O1CCOCC1>[ClH:32].[NH:8]1[CH2:9][CH2:10][CH:11]([NH:14][C:15]2[CH:20]=[CH:19][C:18]([C:21]([F:23])([F:22])[F:24])=[CH:17][N:16]=2)[CH2:12][CH2:13]1.[ClH:32]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 313Hydrochloric AcidHCID 6422Trifluoroacetic acidHCID 58576452tert-Butyl 4-(5-(trifluoromethyl)pyridin-2-ylamino)piperidine-1-carboxylate

生成物 2

HCID 313Hydrochloric AcidHCID 66671897HCID 66671897、化合物

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒2 回
HCID 312751,4-Dioxane溶媒2 回

実験手順

4-(5-Trifluoromethyl-pyridin-2-ylamino)-piperidine-1-carboxylic acid tert-butyl ester (460 mg; 1.33 mmol, prepared in accordance with Example 49) is dissolved in dichloromethane (6 mL) and trifluoroacetic acid (1 mL) is added under stirring. After 30 minutes reaction time, the solution is concentrated under reduced pressure and the residue obtained is co-evaporated with dichloromethane (5 mL). The product isolated is dissolved in dioxane (2 mL) and a 4N solution of hydrochloric acid in dioxane (3 mL) is added. The precipitate formed is filtered, rapidly rinsed with a small amount of dioxane and is dried under high vacuum to afford the desired product as hydrochloride (352 mg; 1.25 mmol).

後処理

  1. customAfter 30 minutes reaction time
  2. concentrationthe solution is concentrated under reduced pressure
  3. customthe residue obtained
  4. customThe product isolated
  5. customThe precipitate formed
  6. filtrationis filtered
  7. washrapidly rinsed with a small amount of dioxane
  8. customis dried under high vacuum

出典と根拠

ORDレコード
ord-9b560bd1b096498e8b4185e815ea1143
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09096524B2

反応ノート

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