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Sodium sulfate decahydrate → tert-butyl (2S,4R)-2-[(dimethylamino)carbonyl]-4-(2-hydroxyethoxy)pyrrolidine-1-carboxylate

HRID 1662718
ノート
印刷プレビュー

反応式

HRID 1662718 の反応式
[CH3:1][N:2]([CH3:24])[C:3]([C@@H:5]1[CH2:9][C@@H:8]([O:10][CH2:11][C:12](OCC)=[O:13])[CH2:7][N:6]1[C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])=[O:4].[H-].[H-].[H-].[H-].[Li+].[Al+3].O.O.O.O.O.O.O.O.O.O.[O-]S([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[CH3:1][N:2]([CH3:24])[C:3]([C@@H:5]1[CH2:9][C@@H:8]([O:10][CH2:11][CH2:12][OH:13])[CH2:7][N:6]1[C:17]([O:19][C:20]([CH3:22])([CH3:21])[CH3:23])=[O:18])=[O:4]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 67430579tert-butyl (2S,4R)-2-[(dimethylamino)carbonyl]-4-(2-ethoxy-2-oxo ethoxy)pyrrolidine-1-carboxylate

生成物 1

HCID 67430889tert-butyl (2S,4R)-2-[(dimethylamino)carbonyl]-4-(2-hydroxyethoxy)pyrrolidine-1-carboxylate収率 115%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

反応条件

温度
-10 °C

実験手順

Under nitrogen atmosphere, to a solution of 2.00 g of the compound obtained in Step 143-1 in THF (40 ml) was added 360 mg of LAH at −40° C., and the reaction mixture was stirred at −10° C. for one hour. To the solution was added sodium sulfate 10 hydrate and the reaction mixture was stirred at room temperature for one hour. The insoluble matter was filtered with celite, the solvent was evaporated under reduced pressure to obtain 2.02 g of the title compound.

後処理

  1. stirringthe reaction mixture was stirred at room temperature for one hour
  2. filtrationThe insoluble matter was filtered with celite
  3. customthe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-45d5fdd74d344f7bbe57cbdfb0509a36
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08030499B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート