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Hydrochloric Acid → 1-[4-(1-Carboxy-1-(3,4-methylenedioxyphenyl)methoxy)phenylmethyl]-2-benzimidazolinone

HRID 274946
ノート
印刷プレビュー

反応式

HRID 274946 の反応式
[C:1]([CH:6]([C:30]1[CH:35]=[CH:34][C:33]2[O:36][CH2:37][O:38][C:32]=2[CH:31]=1)[O:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14][N:15]2[C:19]3[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=3[N:17](C(OCC)=O)[C:16]2=[O:29])=[CH:10][CH:9]=1)([O:3]CC)=[O:2].C(O)C.[OH-].[Na+].Cl>C(Cl)Cl>[C:1]([CH:6]([C:30]1[CH:35]=[CH:34][C:33]2[O:36][CH2:37][O:38][C:32]=2[CH:31]=1)[O:7][C:8]1[CH:9]=[CH:10][C:11]([CH2:14][N:15]2[C:19]3[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=3[NH:17][C:16]2=[O:29])=[CH:12][CH:13]=1)([OH:3])=[O:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 14798Sodium HydroxideHCID 200891941-[4-(1-Carboethoxy-1-(3,4-methylenedioxyphenyl)methoxy)phenylmethyl]-3-carboethoxy-2-benzimidazolinone

生成物 1

HCID 152317851-[4-(1-Carboxy-1-(3,4-methylenedioxyphenyl)methoxy)phenylmethyl]-2-benzimidazolinone収率 80%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A round bottom flask was charged with 0.025 g (0.05 mmol) of the product of step C, 0.5 mL of ethanol and the flask and its contents were placed in a sonicator bath. Methylene chloride (0.3 mL) was then added in order to completely dissolve the starting material. Next, 20 μL of a 5.0 N solution of sodium hydroxide were added and the reaction was stirred at room temperature overnight. The reaction mixture was then adjusted to pH=5 with dropwise addition of 6 N hydrochloric acid, and then concentrated in vacuo. The residue was suspended in water to dissolve inorganic salts and filtered. The flitrate was washed with methanol and dried in vacuo to afford 0.016 g (80%) of the title compound.

後処理

  1. customthe flask and its contents were placed in a sonicator bath
  2. dissolutionto completely dissolve the starting material
  3. concentrationconcentrated in vacuo
  4. dissolutionto dissolve inorganic salts
  5. filtrationfiltered
  6. washThe flitrate was washed with methanol
  7. customdried in vacuo

出典と根拠

ORDレコード
ord-0eaa91c4beed481494f16705c39b709b
出典データセット
uspto-grants-1995_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05391566

反応ノート

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