Sulfuric Acid → HCID 59164407, 화합물

HRID 906590노트

반응식

HRID 906590 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-91f1810d21744b32a3422afca8d23446
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08012988B2

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