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

HRID 1662718
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HRID 1662718 반응식
[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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

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온도
-10 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-45d5fdd74d344f7bbe57cbdfb0509a36
출처 데이터셋
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08030499B2

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