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Hydrochloric Acid → HCID 14722395, 화합물

HRID 1031682
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HRID 1031682 반응식
[C:1](OC(=O)C)(=[O:3])[CH3:2].[OH:8][C:9]1[CH:22]=[C:21]([NH:23][S:24]([CH3:27])(=[O:26])=[O:25])[C:20]([O:28][C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)=[CH:19][C:10]=1[C:11]([CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])=[O:12].[C:35]([O-])(=O)[CH3:36].[Na+].Cl>O.C(OCC)(=O)C>[C:1]([N:23]([C:21]1[C:20]([O:28][C:29]2[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=2)=[CH:19][C:10]2[C:11](=[O:12])[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[C:35]([CH3:36])[O:8][C:9]=2[CH:22]=1)[S:24]([CH3:27])(=[O:26])=[O:25])(=[O:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 7918Acetic AnhydrideHCID 517045Sodium AcetateHCID 10620577HCID 10620577, 화합물

생성물 1

HCID 14722395HCID 14722395, 화합물수율 55.6%

시약·촉매·용매 2

HCID 962Water용매
HCID 8857
Ethyl Acetate
용매

실험 절차

2.55 ml of acetic anhydride was added to 850 mg of ethyl 2-(2-hydroxy-4-methylsulfonylamino-5-phenoxybenzoyl)acetate and 540 mg of sodium acetate. The mixture was stirred for 10 minutes at 110°-120° C. The reaction mixture was introduced into a mixture of 20 ml of ethyl acetate and 20 ml of water. The resulting mixture was adjusted to pH 2 with 2N hydrochloric acid. The organic layer was separated, washed with water and a saturated aqueous sodium chloride solution in this order, and dried with anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure. The residue was purified by a column chromatography (eluant: a 5 : 1 mixture of toluene and ethyl acetate) to obtain 550 mg (yield: 55.6%) of 7-(N-acetyl-N-methylsulfonylamino)-3-ethoxycarbonyl-2-methyl-6-phenoxy-4H-1-benzopyran-4-one.

후처리

  1. customThe organic layer was separated
  2. washwashed with water
  3. dry with materiala saturated aqueous sodium chloride solution in this order, and dried with anhydrous magnesium sulfate
  4. customThe solvent was removed by distillation under reduced pressure
  5. customThe residue was purified by a column chromatography (eluant
  6. additiona 5 : 1 mixture of toluene and ethyl acetate)

출처 및 근거

ORD 기록
ord-a431ed6f23544814a75aebda73c6481c
출처 데이터셋
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04954518

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