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

HRID 61807

反応式

HRID 61807 の反応式
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

参加物

6

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-bbe0e4ef51854def959a91d02be34b07
出典データセット
uspto-grants-2016_09
特許番号
US09440922B2

関連ノート

読み込み中…