1,4-Dioxane hydrochloride → (R)-7,7-difluoro-5-methyl-4-(piperazin-1-yl)-6,7-dihydro-5H-cyclopenta[d]pyrimidine dihydrochloride

HRID 1480577ノート

反応式

HRID 1480577 の反応式
[ClH:1].O1CCOCC1.[F:8][C:9]1([F:32])[C:13]2[N:14]=[CH:15][N:16]=[C:17]([N:18]3[CH2:23][CH2:22][N:21](C(OC(C)(C)C)=O)[CH2:20][CH2:19]3)[C:12]=2[C@H:11]([CH3:31])[CH2:10]1>O1CCOCC1>[ClH:1].[ClH:1].[F:32][C:9]1([F:8])[C:13]2[N:14]=[CH:15][N:16]=[C:17]([N:18]3[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]3)[C:12]=2[C@H:11]([CH3:31])[CH2:10]1

参加物

4

反応物 2

HCID 204431481,4-Dioxane hydrochlorideHCID 66845040HCID 66845040、化合物

生成物 1

HCID 66846210(R)-7,7-difluoro-5-methyl-4-(piperazin-1-yl)-6,7-dihydro-5H-cyclopenta[d]pyrimidine dihydrochloride収率 93%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

4M HCl/dioxane (2.27 mL, 9.09 mmol) was added to a solution of (R)-tert-butyl 4-(7,7-difluoro-5-methyl-6,7-dihydro-5H-cyclopenta[d]pyrimidin-4-yl)piperazine-1-carboxylate (0.092 g, 0.260 mmol) in dioxane (2 mL.) The reaction mixture was stirred at room temperature overnight, after which it was concentrated to dryness and dried on under high vacuum to give (R)-7,7-difluoro-5-methyl-4-(piperazin-1-yl)-6,7-dihydro-5H-cyclopenta[d]pyrimidine dihydrochloride (0.079 g, 93.0% yield) as a solid.

後処理

  1. concentrationafter which it was concentrated to dryness
  2. customdried on under high vacuum

出典と根拠

ORDレコード
ord-f656aabb48204effb85baf85bc37d3aa
出典データセット
uspto-grants-2016_08
特許番号
US09409886B2

反応ノート

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