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Hydrochloric Acid → 1-{2-Amino-6-[(2-aminoethyl)amino]pyridin-3-yl}-2,2,2-trifluoroethanone hydrochloride

HRID 2088650
ノート
印刷プレビュー

反応式

HRID 2088650 の反応式
C(OC(=O)[NH:7][C:8]1[C:13]([C:14](=[O:19])[C:15]([F:18])([F:17])[F:16])=[CH:12][CH:11]=[C:10]([NH:20][CH2:21][CH2:22][NH:23]C(OC(C)(C)C)=O)[N:9]=1)(C)(C)C.[ClH:32]>O1CCOCC1>[ClH:32].[NH2:7][C:8]1[C:13]([C:14](=[O:19])[C:15]([F:16])([F:18])[F:17])=[CH:12][CH:11]=[C:10]([NH:20][CH2:21][CH2:22][NH2:23])[N:9]=1
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 57911745tert-Butyl [6-({2-[(tert-butoxycarbonyl)amino]ethyl}amino)-3-(trifluoroacetyl)pyridin-2-yl]carbamate

生成物 1

HCID 670603221-{2-Amino-6-[(2-aminoethyl)amino]pyridin-3-yl}-2,2,2-trifluoroethanone hydrochloride

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

2.5 g (5.57 mmol) of tert-butyl-[6-({2-[(tert-butoxycarbonyl)amino]ethyl}amino)-3-(trifluoroacetyl)-pyridin-2-yl]carbamate (Example 12A) were dissolved in 15 ml of a 4 N solution of hydrogen chloride in dioxane and stirred for 20 h. The reaction mixture was concentrated to half of its original volume, and the same amount of diethyl ether was added. The reaction mixture was stirred for 20 min, and the product was filtered off and washed with diethyl ether. This gave 1.4 g (89% of theory) of the product as a solid.

後処理

  1. concentrationThe reaction mixture was concentrated to half of its original volume
  2. additionthe same amount of diethyl ether was added
  3. stirringThe reaction mixture was stirred for 20 min
  4. filtrationthe product was filtered off
  5. washwashed with diethyl ether

出典と根拠

ORDレコード
ord-8c30299eaf8d4d4daa4afe973858670f
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08436003B2

反応ノート

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