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Methanol → methyl 2-((2R)-pyrrolidin-2-yl)acetate hydrochloride

HRID 2111439
ノート
印刷プレビュー

反応式

HRID 2111439 の反応式
Cl.[NH:2]1[CH2:10][CH2:9][CH2:8][C@@H:3]1[CH2:4][C:5]([OH:7])=[O:6].S(Cl)([Cl:13])=O.[CH3:15]O>>[ClH:13].[CH3:15][O:6][C:5](=[O:7])[CH2:4][C@H:3]1[CH2:8][CH2:9][CH2:10][NH:2]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 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 45026933(R)-2-(Pyrrolidin-2-yl)acetic acid hydrochloride

生成物 1

HCID 68738055methyl 2-((2R)-pyrrolidin-2-yl)acetate hydrochloride

実験手順

To a solution of 2.0 g (0.012 mole) of D-beta-homoproline hydrochloride in 20 mL of methanol was added slowly 1.8 mL (0.024 mole) of thionyl chloride at 0 degrees. The mixture was stirred overnight, then concentrated under reduced pressure. The solid was slurried in ether, and collected by filtration to give 2.2 g of (2R)-pyrrolidin-2-yl-acetic acid methyl ester hydrochloride as a white solid. A solution of 2.2 g (0.012 mole) of (2R)-pyrrolidin-2-yl-acetic acid methyl ester hydrochloride in 3 mL of chloroform was added over 5 minutes to a cooled (0 degrees) mixture of 2.34 g (0.012 mole) of 2,4-dichloro-5-nitro-pyrimidine, 5.1 g (0.060 mole) of sodium bicarbonate and 25 mL of ethyl acetate. The cooling bath was removed and the mixture stirred for 17 hours at room temperature. Activated charcoal was added and after stirring briefly, the mixture was filtered through a pad of Celite, washing the filter pad with ethyl acetate. The filtrate was concentrated under reduced pressure. Purification of the residue by silica gel chromatography, eluting with hexanes-ethyl acetate (100:0-70:30) gave 3.3 g of [(R)-1-(2-chloro-5-nitro-pyrimidin-4-yl)-pyrrolidin-2-yl]-acetic acid methyl ester (IV-102) as a yellow thick oil.

後処理

  1. concentrationconcentrated under reduced pressure
  2. filtrationcollected by filtration

出典と根拠

ORDレコード
ord-a6148a2c59f145e795527c8aea1a1b08
出典データセット
uspto-grants-2009_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07517873B2

反応ノート

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