Water → 6-Methoxy-3,4-dihydro-2H-1,4-benzoxazine

HRID 1167609ノート

反応式

HRID 1167609 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[O:11][CH2:10][CH2:9][N:8](C(=O)C)[C:7]=2[CH:15]=1.O.[OH-].[K+]>CO>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[O:11][CH2:10][CH2:9][NH:8][C:7]=2[CH:15]=1

参加物

5

反応物 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 22993340HCID 22993340、化合物

生成物 1

HCID 162444606-Methoxy-3,4-dihydro-2H-1,4-benzoxazine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
60 °C

実験手順

The compound obtained in Step C (1.5 g; 7.26 mmol) is dissolved in 7 ml of methanol, and then water (14 eq.; 101.6 mmol; 1.9 ml) and potassium hydroxide (6 eq.; 43.5 mmol; 2.44 g) are added. The solution is stirred vigorously at 60° C. for 2 hours. After extraction three times with dichloromethane, the organic phase is dried over MgSO4 and then removed under reduced pressure. The residue obained is purified by flash chromatography on silica gel (eluant: PE/AcOEt (1/1)). The title product is obtained in the form of a red solid.

後処理

  1. extractionAfter extraction three times with dichloromethane
  2. dry with materialthe organic phase is dried over MgSO4
  3. customremoved under reduced pressure
  4. customThe residue obained is purified by flash chromatography on silica gel (eluant: PE/AcOEt (1/1))

出典と根拠

ORDレコード
ord-f087d9ce4ece467bbf58fbc696f21d80
出典データセット
uspto-grants-2003_09
特許番号
US06620809B2

反応ノート

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