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

HRID 1167609노트

반응식

HRID 1167609 반응식
[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

참가 물질

5

반응물 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 22993340HCID 22993340, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
60 °C

실험 절차

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.

후처리

  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))

출처 및 근거

ORD 기록
ord-f087d9ce4ece467bbf58fbc696f21d80
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06620809B2

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