Ammonium Hydroxide → 6-bromo-8-methoxy-4,4-dimethyl-1,4-dihydro-2H-3,1-benzoxazin-2-one

HRID 50736

반응식

HRID 50736 반응식
[CH3:1][O:2][C:3]1[C:12]2[NH:11][C:10](=[O:13])[O:9][C:8]([CH3:15])([CH3:14])[C:7]=2[CH:6]=[CH:5][CH:4]=1.C([O-])(=O)C.[Na+].[Br:21]Br.[OH-].[NH4+]>C(O)(=O)C>[Br:21][C:5]1[CH:4]=[C:3]([O:2][CH3:1])[C:12]2[NH:11][C:10](=[O:13])[O:9][C:8]([CH3:15])([CH3:14])[C:7]=2[CH:6]=1

참가 물질

6

반응물 4

HCID 14923Ammonium HydroxideHCID 24408BromineHCID 2106172H-3,1-Benzoxazin-2-one, 1,4-dihydro-4,4-dimethyl-8-methoxy-HCID 517045Sodium Acetate

생성물 1

HCID 235096426-bromo-8-methoxy-4,4-dimethyl-1,4-dihydro-2H-3,1-benzoxazin-2-one수율 93.4%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

To a mixture of 8-methoxy-4,4-dimethyl-1,4-dihydro-2H-3,1-benzoxazin-2-one (2.1 g, 10.1 mmol), sodium acetate (1.5 g, 18 mmol) in acetic acid (30 mL) was added bromine (0.62 mL, 12 mmol) at ambient temperature. After 30 minutes, the solution was treated with a concentrated ammonium hydroxide solution (50 mL). The precipitate was collected on a filter and washed with water (3×20 mL) to yield 6-bromo-8-methoxy-4,4-dimethyl-1,4-dihydro-2H-3,1-benzoxazin-2-one (2.7 g, 93%) as off-white solid: MS (ESI) m/z 286, 288 [M+H]+.

후처리

  1. customThe precipitate was collected on
  2. filtrationa filter
  3. washwashed with water (3×20 mL)

출처 및 근거

ORD 기록
ord-57356ea393df435c9d4c129165c98866
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06713478B2

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