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Sodium periodate → Benzyl 4-[1-(ethoxycarbonyl)-3-oxopropyl]piperidine-1-carboxylate

HRID 1725644
ノート
印刷プレビュー

反応式

HRID 1725644 の反応式
[CH2:1]([O:3][C:4]([CH:6]([CH:10]1[CH2:15][CH2:14][N:13]([C:16]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[O:17])[CH2:12][CH2:11]1)[CH2:7][CH:8]=C)=[O:5])[CH3:2].I([O-])(=O)(=O)=[O:27].[Na+]>C1COCC1.O.[O-]S([O-])=O.[Na+].[Na+].C([O-])(O)=O.[Na+].[Os](=O)(=O)(=O)=O>[CH2:1]([O:3][C:4]([CH:6]([CH:10]1[CH2:15][CH2:14][N:13]([C:16]([O:18][CH2:19][C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)=[O:17])[CH2:12][CH2:11]1)[CH2:7][CH:8]=[O:27])=[O:5])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 2

HCID 23667635Sodium periodateHCID 67441606Ethyl 1-[(phenylmethoxy)carbonyl]-α-2-propen-1-yl-4-piperidineacetate

生成物 1

HCID 86616780Benzyl 4-[1-(ethoxycarbonyl)-3-oxopropyl]piperidine-1-carboxylate収率 58.3%

試薬・触媒・溶媒 5

HCID 30318Osmium Tetroxide触媒HCID 962Water溶媒
HCID 8028
Tetrahydrofuran
溶媒
HCID 24437Sodium Sulfite溶媒
HCID 516892Sodium Bicarbonate溶媒

実験手順

Benzyl 4-[1-(ethoxycarbonyl)but-3-en-1-yl]piperidine-1-carboxylate (4.08 g, 11.8 mmol) was dissolved in THF (45 mL), and osmium tetroxide (0.45 mL, 2.5% solution in t-butanol) was added followed by a solution of sodium periodate (7.57 g, 35.4 mmol) in water (37 mL). After 24 h, the reaction was diluted with saturated aqueous Na2SO3 and NaHCO3 and extracted with ethyl acetate (4×). The combined organic washes were dried over sodium sulfate, filtered and evaporated. The crude product was purified by silica gel chromatography, eluting with a gradient of 50 to 100% EtOAc:hexanes to give the title compound (2.39 g). MS: m/z=348.1 (M+1).

後処理

  1. extractionextracted with ethyl acetate (4×)
  2. dry with materialThe combined organic washes were dried over sodium sulfate
  3. filtrationfiltered
  4. customevaporated
  5. customThe crude product was purified by silica gel chromatography
  6. washeluting with a gradient of 50 to 100% EtOAc

出典と根拠

ORDレコード
ord-1ffed2019c9f4afeba41589828126113
出典データセット
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07491713B2

反応ノート

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