Sulfuric Acid → HCID 59164407, 화합물

HRID 1441615노트

반응식

HRID 1441615 반응식
[CH3:1][O:2][C:3](=[O:16])[C:4]1[CH:9]=[CH:8][C:7]([CH2:10][F:11])=[CH:6][C:5]=1[NH:12]C(=O)C.S(=O)(=O)(O)O>CO>[CH3:1][O:2][C:3](=[O:16])[C:4]1[CH:9]=[CH:8][C:7]([CH2:10][F:11])=[CH:6][C:5]=1[NH2:12]

참가 물질

4

반응물 2

HCID 1118Sulfuric AcidHCID 59164463HCID 59164463, 화합물

생성물 1

HCID 59164407HCID 59164407, 화합물수율 101.6%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 2-acetylamino-4-fluoromethyl-benzoic acid methyl ester (1.5 g, 6.66 equiv) in MeOH (50 mL) was added concd sulfuric acid (4 mL) and the mixture was refluxed for 1 h. The mixture was cooled down and concentrated in vacuo. Water was added and the pH was adjusted to 9-10 by addition of 2N NaOH. The aqueous phase was extracted with AcOEt. The organic phase were combined, washed with brine and dried (Na2SO4). The solution was concentrated in vacuo to afford the title compound as a yellow-orange oil (1.24 g, 100%) (ES-MS: m/z 184.1 [M+H]+, rt 4.91 min).

후처리

  1. temperaturethe mixture was refluxed for 1 h
  2. temperatureThe mixture was cooled down
  3. concentrationconcentrated in vacuo
  4. additionWater was added
  5. additionthe pH was adjusted to 9-10 by addition of 2N NaOH
  6. extractionThe aqueous phase was extracted with AcOEt
  7. washwashed with brine
  8. dry with materialdried (Na2SO4)
  9. concentrationThe solution was concentrated in vacuo

출처 및 근거

ORD 기록
ord-b8343c6d61344f448857a650209ad452
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07655666B2

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