Ammonium Hydroxide → 3-Hydroxydodecanamide

HRID 1872800노트

반응식

HRID 1872800 반응식
[OH:1][CH:2]([CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15])[CH2:3][C:4](O)=[O:5].Cl.C([N:19]=C=NCCCN(C)C)C.ON1C2C=CC=CC=2N=N1.[OH-].[NH4+]>O1CCCC1.C(OCC)(=O)C>[OH:1][CH:2]([CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15])[CH2:3][C:4]([NH2:19])=[O:5]

참가 물질

7

반응물 4

HCID 14923Ammonium HydroxideHCID 757711-HydroxybenzotriazoleHCID 94216(+-)-3-Hydroxydodecanoic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

생성물 1

HCID 186873013-Hydroxydodecanamide수율 98.9%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 3-hydroxydodecanoic acid (0.26 g) in tetrahydrofuran (4 ml) was added 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (0.18 g) and 1-hydroxybenzotriazole (0.24 g). After stirring for 30 minutes, 28% ammonium hydroxide (0.17 ml) was added and the mixture was stirred at room temperature overnight. Then, the mixture was diluted with ethyl acetate (100 ml) and washed with 0.1 N-hydrochloric acid (100 ml×2), saturated sodium bicarbonate (50 ml), and brine (50 ml). After drying over magnesium sulfate and evaporation, the residue was recrystallized from isopropyl alcohol (1 ml) to give 3-hydroxydodecanamide (0.20 g).

후처리

  1. stirringthe mixture was stirred at room temperature overnight
  2. washwashed with 0.1 N-hydrochloric acid (100 ml×2), saturated sodium bicarbonate (50 ml), and brine (50 ml)
  3. dry with materialAfter drying over magnesium sulfate and evaporation
  4. customthe residue was recrystallized from isopropyl alcohol (1 ml)

출처 및 근거

ORD 기록
ord-e2e7252397d045e385e6c22256d35e6c
출처 데이터셋
uspto-grants-2000_08
특허 번호
US06110933

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