Water → Methyl 2-amino-4-iodobenzoate

HRID 1449568노트

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HRID 1449568 반응식
[OH-].[Na+].[I:3][C:4]1[CH:15]=[CH:14][C:7]2[C:8](=[O:13])[O:9][C:10](=O)[NH:11][C:6]=2[CH:5]=1.O>CO>[NH2:11][C:6]1[CH:5]=[C:4]([I:3])[CH:15]=[CH:14][C:7]=1[C:8]([O:9][CH3:10])=[O:13]

참가 물질

5

반응물 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 189299207-Iodo-1H-benzo[d][1,3]oxazine-2,4-dione

생성물 1

HCID 18929930Methyl 2-amino-4-iodobenzoate수율 80.2%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
60 °C

실험 절차

To a stirred solution of sodium hydroxide (0.048 g, 1.2 mM) in methanol (4.5 mL) was added 7-iodo-2H-3,1-benzoxazine-2,4(1H)-dione (2.6 g, 9.0 mM). The mixture was heated at 60° C. for 7 hr and the resulting solution was cooled, poured into water and extracted with ethyl acetate. The combined extracts were washed once with dilute sodium hydroxide, dried (MgSO4), filtered and concentrated to leave the title compound (2.0 g, 80%) as a brown oil which slowly crystallized; MS(CI): 278 (M+H).

후처리

  1. temperaturethe resulting solution was cooled
  2. extractionextracted with ethyl acetate
  3. washThe combined extracts were washed once with dilute sodium hydroxide
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-3f38d9f3a4bf446695c35c493e5c313e
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05599814

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