Lithium hydroxide, monohydrate → 4-Iodocinnamic acid

HRID 1765696노트

반응식

HRID 1765696 반응식
C([O:3][C:4](=[O:14])[CH:5]=[CH:6][C:7]1[CH:12]=[CH:11][C:10]([I:13])=[CH:9][CH:8]=1)C.O.[OH-].[Li+]>CO.O1CCCC1.O>[I:13][C:10]1[CH:9]=[CH:8][C:7]([CH:6]=[CH:5][C:4]([OH:14])=[O:3])=[CH:12][CH:11]=1

참가 물질

6

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 541932622-Propenoic acid, 3-(4-iodophenyl)-, ethyl ester

생성물 1

HCID 35997884-Iodocinnamic acid수율 100.8%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of ethyl-4-iodo-cinnamate (3.2 g, 10.5 mmol) in methanol (25 mL), tetrahydrofuran (25 ml) and water (15 mL) was treated with lithium hydroxide monohydrate (4.2 g, 100 mmol) and the resulting reaction mixture was stirred at ambient temperature over 2 days. The volatiles were evaporated in vacuo and the residue was neutralized with saturated aqueous ammonium chloride solution. The precipitated solid was filtered, washed with water and hexane and dried to afford the title product as a white solid (2.9 g, 91%). It was used as such for the next step.

후처리

  1. customthe resulting reaction mixture
  2. customThe volatiles were evaporated in vacuo
  3. filtrationThe precipitated solid was filtered
  4. washwashed with water and hexane
  5. customdried

출처 및 근거

ORD 기록
ord-3fa7d1401703467d9dce94703be8a54e
출처 데이터셋
uspto-grants-2007_06
특허 번호
US07226951B2

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