Magnesium Bromide → (5-hydroxy-4-oxoquinazolin-3(4H)-yl)methyl pivalate

HRID 1162206노트

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HRID 1162206 반응식
[Br-].[Mg+2].[Br-].[C:4]([O:10][CH2:11][N:12]1[C:21](=[O:22])[C:20]2[C:15](=[CH:16][CH:17]=[CH:18][C:19]=2[O:23]C)[N:14]=[CH:13]1)(=[O:9])[C:5]([CH3:8])([CH3:7])[CH3:6]>N1C=CC=CC=1>[C:4]([O:10][CH2:11][N:12]1[C:21](=[O:22])[C:20]2[C:15](=[CH:16][CH:17]=[CH:18][C:19]=2[OH:23])[N:14]=[CH:13]1)(=[O:9])[C:5]([CH3:8])([CH3:7])[CH3:6]

참가 물질

4

반응물 2

HCID 82241Magnesium BromideHCID 68496089(5-methoxy-4-oxoquinazolin-3(4H)-yl)methyl pivalate

생성물 1

HCID 68496163(5-hydroxy-4-oxoquinazolin-3(4H)-yl)methyl pivalate수율 90%

시약·촉매·용매 1

HCID 1049Pyridine용매

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온도
120 °C

실험 절차

Magnesium bromide (7 g, 38 mmol) was added to a solution of (5-methoxy-4-oxoquinazolin-3(4H)-yl)methyl pivalate (7.4 g, 25.5 mmol) in pyridine (25 ml). The mixture was stirred at 120° C. for one hour. After cooling, the solvents were evaporated under high vacuum. Diluted acetic acid (15 ml in 100 ml water) was added. The precipitated solid was filtered, washed with water and dried under high vacuum in the presence of P2O5 to give (5-hydroxy-4-oxoquinazolin-3(4H)-yl)methyl pivalate as a white solid (6.33 g, 90%); NMR Spectrum (CDCl3) 1.23 (s, 9H), 5.93 (s, 2H), 6.99 (d, 1H), 7.22 (d, 1H), 7.68 (t, 1H), 8.21 (s, 1H); Mass spectrum MH+ 277.

후처리

  1. temperatureAfter cooling
  2. customthe solvents were evaporated under high vacuum
  3. additionDiluted acetic acid (15 ml in 100 ml water) was added
  4. filtrationThe precipitated solid was filtered
  5. washwashed with water
  6. dry with materialdried under high vacuum in the presence of P2O5

출처 및 근거

ORD 기록
ord-b8c087fcad29492e82b2efb28a7aa7e8
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07820683B2

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