Methanol → 4-{[4-(2,3-Dihydroxypropoxy)phenyl]ethynyl}benzoic acid

HRID 1519689노트

반응식

HRID 1519689 반응식
[OH-].[Na+].C1COCC1.CO.[OH:10][CH:11]([CH2:32][OH:33])[CH2:12][O:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]#[C:21][C:22]2[CH:31]=[CH:30][C:25]([C:26]([O:28]C)=[O:27])=[CH:24][CH:23]=2)=[CH:16][CH:15]=1>C(O)(=O)C>[OH:10][CH:11]([CH2:32][OH:33])[CH2:12][O:13][C:14]1[CH:15]=[CH:16][C:17]([C:20]#[C:21][C:22]2[CH:23]=[CH:24][C:25]([C:26]([OH:28])=[O:27])=[CH:30][CH:31]=2)=[CH:18][CH:19]=1

참가 물질

6

반응물 4

HCID 887MethanolHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 71268214Methyl 4-{[4-(2,3-dihydroxypropoxy)phenyl]ethynyl}benzoate

생성물 1

HCID 712681454-{[4-(2,3-Dihydroxypropoxy)phenyl]ethynyl}benzoic acid수율 91%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A 10% aqueous solution (5.5 mL) of sodium hydroxide was added to a THF (25 mL)-MeOH (15 mL) solution of methyl 4-{[4-(2,3-dihydroxypropoxy)phenyl]ethynyl}benzoate (0.92 g) as obtained in Example 11-(1), and the mixture was stirred for 3.5 hours at room temperature. Then, acetic acid (1.2 mL) was added for neutralization. The reaction mixture was concentrated, and water was added. The precipitated solid was filtered off and dried to obtain 4-{[4-(2,3-dihydroxypropoxy)phenyl]ethynyl}benzoic acid (light green solid) (0.80 g, 91%).

후처리

  1. customas obtained in Example 11-(1)
  2. concentrationThe reaction mixture was concentrated
  3. additionwater was added
  4. filtrationThe precipitated solid was filtered off
  5. customdried

출처 및 근거

ORD 기록
ord-a7ccaf297dc34a1099a78329c4143990
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09073821B2

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