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Methanol → 5-Tert-butyl 2-methyl 6,7-dihydrooxazolo[5,4-C]pyridine-2,5(4H)-dicarboxylate

HRID 546402
ノート
印刷プレビュー

反応式

HRID 546402 の反応式
[C-]#N.[Na+].[C:4]([O:8][C:9]([N:11]1[CH2:16][CH2:15][C:14]2[N:17]=[C:18]([CH:20]=[O:21])[O:19][C:13]=2[CH2:12]1)=[O:10])([CH3:7])([CH3:6])[CH3:5].[CH3:22][OH:23]>[O-2].[O-2].[Mn+4]>[C:4]([O:8][C:9]([N:11]1[CH2:16][CH2:15][C:14]2[N:17]=[C:18]([C:20]([O:23][CH3:22])=[O:21])[O:19][C:13]=2[CH2:12]1)=[O:10])([CH3:7])([CH3:5])[CH3:6]
参加物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 887MethanolHCID 8929Sodium CyanideHCID 17842499HCID 17842499、化合物

生成物 1

HCID 178424645-Tert-butyl 2-methyl 6,7-dihydrooxazolo[5,4-C]pyridine-2,5(4H)-dicarboxylate

試薬・触媒・溶媒 1

HCID 178418406HCID 178418406、化合物触媒

実験手順

Sodium cyanide (220 mg) and manganese dioxide (780 mg) were added to a solution of 5-(tert-butoxycarbonyl)-2-formyl-4,5,6,7-tetrahydrooxazolo[5,4-c]pyridine (225 mg) in methanol (9.0 ml) at room temperature. After stirring for 30 minutes, the reaction mixture was filtered through Celite with ethyl acetate. The filtrate was washed with water (50 ml) and saturated saline (50 ml) and dried over anhydrous sodium sulfate. The solvent was then distilled off under reduced pressure, and the residue was purified by column chromatography on silica gel (hexane:ethyl acetate=3:2→1:1) to obtain the title compound (120 mg) as a colorless amorphous substance.

後処理

  1. filtrationthe reaction mixture was filtered through Celite with ethyl acetate
  2. washThe filtrate was washed with water (50 ml) and saturated saline (50 ml)
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationThe solvent was then distilled off under reduced pressure
  5. customthe residue was purified by column chromatography on silica gel (hexane:ethyl acetate=3:2→1:1)

出典と根拠

ORDレコード
ord-20283ff79af8481ca1a691241dbc9c8c
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07935824B2

反応ノート

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