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Sodium Hydroxide → 2-[[(8-chlorodibenz[b,f][1,4]oxazepin-10(11H)-yl)carbonyl]amino]acetic acid

HRID 2258440
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HRID 2258440 반응식
[Cl:1][C:2]1[CH:25]=[CH:24][C:5]2[O:6][C:7]3[CH:23]=[CH:22][CH:21]=[CH:20][C:8]=3[CH2:9][N:10]([C:11]([NH:13][CH2:14][C:15]([O:17]CC)=[O:16])=[O:12])[C:4]=2[CH:3]=1.[OH-].[Na+]>CO>[Cl:1][C:2]1[CH:25]=[CH:24][C:5]2[O:6][C:7]3[CH:23]=[CH:22][CH:21]=[CH:20][C:8]=3[CH2:9][N:10]([C:11]([NH:13][CH2:14][C:15]([OH:17])=[O:16])=[O:12])[C:4]=2[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium Hydroxide2회HCID 10570547HCID 10570547, 화합물

생성물 1

HCID 108304472-[[(8-chlorodibenz[b,f][1,4]oxazepin-10(11H)-yl)carbonyl]amino]acetic acid수율 99.5%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To the product of Example 3 (5.1 g, 14.2 mmol) dissolved in 100 mL of methanol (MeOH) was added 25 mL (25.0 mmol) of 1N sodium hydroxide. (NaOH). This reaction was stirred at room temperature overnight before all solvent was removed under reduced pressure. The residue was dissolved in 250 mL of water and the solution was brought to pH 3 with 1N HCl. The product was extracted from the aqueous phase with 3×250 mL of Et2O. The Et2O layer was then dried (Na2SO4), filtered, and stripped of all solvent under reduced pressure to provide 4.7 g of the title compound after drying in a vacuum oven.

후처리

  1. customwas removed under reduced pressure
  2. dissolutionThe residue was dissolved in 250 mL of water
  3. extractionThe product was extracted from the aqueous phase with 3×250 mL of Et2O
  4. dry with materialThe Et2O layer was then dried (Na2SO4)
  5. filtrationfiltered

출처 및 근거

ORD 기록
ord-74e6acb4a2ab44409881aa3291a9b1ff
출처 데이터셋
uspto-grants-1997_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05661146

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