Methanol → HCID 21941479、化合物

HRID 1158925ノート

反応式

HRID 1158925 の反応式
[N:1]1[N:9]2[C:4]([O:5][CH2:6][CH2:7][CH2:8]2)=[CH:3][C:2]=1[C:10]([O-])=[O:11].[BH4-].[Li+].CO>C1COCC1>[NH:1]1[N:9]2[CH:4]([O:5][CH2:6][CH:7]=[CH:8]2)[CH2:3][CH:2]1[CH2:10][OH:11]

参加物

5

反応物 3

HCID 887MethanolHCID 4148881Lithium borohydrideHCID 21941385HCID 21941385、化合物

生成物 1

HCID 21941479HCID 21941479、化合物収率 67%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To the stirred solution of 6,7-dihydro-5H-pyrazolo[5,1-b][1,3]oxazine-2-carboxylate: (4.0 g, 20 mmol) of in 100 ml of THF was added 0.71 g of lithium borohydride and 1.03 g of methanol. The solution was heated at 40 C for 2.5 hour. The reaction was quenched by 1N HCl, and adjusted to pH 1.3 and stirred at room temperature for 1 hour. The reaction mixture was adjusted pH to 8 with k2CO3. The reaction mixture was extracted with ethyl acetate. The organic layer was dried over MgSO4, and concentrated to an oil and column chromatographed to give 2.08 g of the desired product (67%); (M+H) 155.

後処理

  1. temperatureThe solution was heated at 40 C for 2.5 hour
  2. customThe reaction was quenched by 1N HCl
  3. extractionThe reaction mixture was extracted with ethyl acetate
  4. dry with materialThe organic layer was dried over MgSO4
  5. concentrationconcentrated to an oil and column
  6. customchromatographed

出典と根拠

ORDレコード
ord-edbc18597cf7451c92e72823fd34df6c
出典データセット
uspto-grants-2010_10
特許番号
US07812014B2

反応ノート

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