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Hydrochloric Acid → (3S*,4R*)-4-(2,4-difluorophenyl)-1-ethylpyrrolidine-3-carboxylic acid hydrochloride

HRID 1992664
ノート
印刷プレビュー

反応式

HRID 1992664 の反応式
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C@@H:9]1[CH2:13][N:12]([CH2:14][CH3:15])[CH2:11][C@H:10]1[C:16]([O:18]C)=[O:17].C[Si](C)(C)[O-].[K+].[ClH:26]>C(OCC)C.O1CCOCC1>[ClH:26].[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C@@H:9]1[CH2:13][N:12]([CH2:14][CH3:15])[CH2:11][C@H:10]1[C:16]([OH:18])=[O:17]
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 3

HCID 313Hydrochloric AcidHCID 23668039Potassium trimethylsilanolateHCID 59130979Methyl (3S*,4R*)-4-(2,4-difluorophenyl)-1-ethylpyrrolidine-3-carboxylate

生成物 1

HCID 67211765(3S*,4R*)-4-(2,4-difluorophenyl)-1-ethylpyrrolidine-3-carboxylic acid hydrochloride

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒
HCID 31275
1,4-Dioxane
溶媒

実験手順

To a stirred solution of methyl (3S,4R)-4-(2,4-difluorophenyl)-1-ethylpyrrolidine-3-carboxylate, from preparation 18 (5.9 g, 22 mmol) in diethyl ether (59 mL) at room temperature under dry nitrogen was added potassium trimethylsilanolate (2.36 g, 26 mmol) in a single portion. The resulting mixture was stirred at room temperature under N2 for 3 hours. A solution of 4M hydrogen chloride in dioxane (20 mL) was then added and the resulting mixture was stirred under dry nitrogen at room temperature for 18 hours, and then concentrated in vacuo to afford the title compound as a white solid containing potassium chloride residues (7.0 g).

後処理

  1. stirringthe resulting mixture was stirred under dry nitrogen at room temperature for 18 hours
  2. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-0c5d2a6130d04a11888bc74d576ad4d7
出典データセット
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07649002B2

反応ノート

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