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

HRID 1918335
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HRID 1918335 반응식
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
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참가 물질

6

반응물 4

HCID 962WaterHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 671703457-(2-m-Tolyl-ethoxy)-benzo[1,3]dioxole-5-carboxylic Acid 2-m-tolyl-ethyl Ester

생성물 1

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

시약·촉매·용매 1

HCID 887
Methanol
용매

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온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e28cc4705674484c91925bc6e53ecd91
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08618304B2

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