Hydrochloric Acid → (3-Bromo-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazol-9-yl oxy)-acetic acid

HRID 61807

반응식

HRID 61807 반응식
C[O:2][C:3](=[O:27])[CH2:4][O:5][C:6]1[CH:26]=[CH:25][C:9]2[C:10]([CH3:24])([CH3:23])[C:11]3[NH:12][C:13]4[C:18]([C:19]=3[C:20](=[O:21])[C:8]=2[CH:7]=1)=[CH:17][CH:16]=[C:15]([Br:22])[CH:14]=4.COC(=O)CO.[OH-].[Na+].Cl>CO>[Br:22][C:15]1[CH:14]=[C:13]2[C:18]([C:19]3[C:20](=[O:21])[C:8]4[CH:7]=[C:6]([O:5][CH2:4][C:3]([OH:27])=[O:2])[CH:26]=[CH:25][C:9]=4[C:10]([CH3:24])([CH3:23])[C:11]=3[NH:12]2)=[CH:17][CH:16]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 66774Methyl GlycolateHCID 66833939(3-bromo-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazol-9-yl oxy)-acetic acid methyl ester

생성물 1

HCID 66834695(3-Bromo-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazol-9-yl oxy)-acetic acid수율 48%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Under the same conditions as the method for synthesizing Compound A7-1, (3-bromo-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazol-9-yl oxy)-acetic acid methyl ester was prepared from Compound JJ2 and hydroxy-acetic acid methyl ester. The resultant was dissolved in MeOH (0.35 ml), added with aqueous solution of sodium hydroxide (6 mol/1), and stirred at room temperature for 10 min. The reaction solution was added with hydrochloric acid (3 mol/1), extracted with diethyl ether and dried over anhydrous magnesium sulfate. After the concentration under reduced pressure, white solid was obtained, which was then washed with methylene chloride to obtain the title compound (11.2 mg, 48%).

후처리

  1. extractionextracted with diethyl ether
  2. dry with materialdried over anhydrous magnesium sulfate
  3. concentrationAfter the concentration under reduced pressure
  4. customwhite solid was obtained
  5. washwhich was then washed with methylene chloride

출처 및 근거

ORD 기록
ord-bbe0e4ef51854def959a91d02be34b07
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09440922B2

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