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Water → 7-(2-m-Tolyl-ethoxy)-benzo[1,3]dioxole-5-carboxylic Acid

HRID 1918335
ノート
印刷プレビュー

反応式

HRID 1918335 の反応式
C1(C)C=CC=C(CC[O:9][C:10]([C:12]2[CH:20]=[C:19]([O:21][CH2:22][CH2:23][C:24]3[CH:25]=[C:26]([CH3:30])[CH:27]=[CH:28][CH:29]=3)[C:15]3[O:16][CH2:17][O:18][C:14]=3[CH:13]=2)=[O:11])C=1.[OH-].[Na+].C1COCC1.O>CO>[C:26]1([CH3:30])[CH:27]=[CH:28][CH:29]=[C:24]([CH2:23][CH2:22][O:21][C:19]2[C:15]3[O:16][CH2:17][O:18][C:14]=3[CH:13]=[C:12]([C:10]([OH:11])=[O:9])[CH:20]=2)[CH:25]=1
参加物反応条件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 962WaterHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 671703457-(2-m-Tolyl-ethoxy)-benzo[1,3]dioxole-5-carboxylic Acid 2-m-tolyl-ethyl Ester

生成物 1

HCID 671702937-(2-m-Tolyl-ethoxy)-benzo[1,3]dioxole-5-carboxylic Acid収率 96%

試薬・触媒・溶媒 1

HCID 887
Methanol
溶媒

反応条件

温度
50 °C

実験手順

4.5 g of 7-(2-m-tolyl-ethoxy)-benzo[1,3]dioxole-5-carboxylic acid 2-m-tolyl-ethyl ester and 650 mg of sodium hydroxide were dissolved in 50 ml of methanol, 50 ml of THF and 5 ml of water. The mixture was kept at room temperature for 20 h, then stirred at 50° C. for 5 h and evaporated. The residue was dissolved in 300 ml of a 0.1 M aqueous solution of sodium hydroxide and washed three times with 50 ml each of diisopropyl ether. The pH was adjusted to 2 with sodium hydrogensulfate and the mixture stirred for 30 min at room temperature. The product was collected by filtration, washed and dried in vacuo to yield 3.1 g of the title compound.

後処理

  1. customevaporated
  2. dissolutionThe residue was dissolved in 300 ml of a 0.1 M aqueous solution of sodium hydroxide
  3. washwashed three times with 50 ml each of diisopropyl ether
  4. stirringthe mixture stirred for 30 min at room temperature
  5. filtrationThe product was collected by filtration
  6. washwashed
  7. customdried in vacuo

出典と根拠

ORDレコード
ord-e28cc4705674484c91925bc6e53ecd91
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08618304B2

反応ノート

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