1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride → HCID 23076606, 화합물

HRID 2221953노트

반응식

HRID 2221953 반응식
Cl.[CH3:2]OCN.[CH3:6][O:7][C:8]1[CH:9]=[C:10]([CH:22]=[CH:23][C:24]=1[O:25][CH2:26][C:27]1[N:28]=[C:29]([C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)[O:30][C:31]=1[CH3:32])[CH2:11][O:12][C:13]1[C:17]([C:18]([OH:20])=O)=[CH:16][N:15]([CH3:21])[N:14]=1.O.[OH:40][N:41]1[C:45]2C=CC=CC=2N=N1.Cl.C(N=C=NCCCN(C)C)C>O.CN(C)C=O.C(N(CC)CC)C>[CH3:2][O:40][N:41]([CH3:45])[C:18]([C:17]1[C:13]([O:12][CH2:11][C:10]2[CH:22]=[CH:23][C:24]([O:25][CH2:26][C:27]3[N:28]=[C:29]([C:33]4[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=4)[O:30][C:31]=3[CH3:32])=[C:8]([O:7][CH3:6])[CH:9]=2)=[N:14][N:15]([CH3:21])[CH:16]=1)=[O:20]

참가 물질

8

반응물 4

HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 21959107Methoxymethanamine hydrochlorideHCID 692152243-{[3-methoxy-4-(5-methyl-2-phenyl-1,3-oxazol-4-ylmethoxy)benzyl]oxy}-1-methyl-1H-pyrazole-4-carboxylic acid

생성물 1

HCID 23076606HCID 23076606, 화합물수율 96%

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8471Triethylamine용매

실험 절차

A mixture of methoxymethylamine hydrochloride (0.85 g), triethylamine (1.3 mL) and N,N-dimethylformamide (20 mL) was stirred at room temperature for 30 min. To the reaction mixture were added 3-{[3-methoxy-4-(5-methyl-2-phenyl-1,3-oxazol-4-ylmethoxy)benzyl]oxy}-1-methyl-1H-pyrazole-4-carboxylic acid (3.45 g), 1-hydroxy-1H-1,2,3-benzotriazole monohydrate (1.22 g) and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (1.60 g), and the mixture was stirred overnight at room temperature. The reaction mixture was poured into water and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed successively with dilute hydrochloric acid, saturated aqueous sodium hydrogen carbonate and saturated brine, dried over anhydrous magnesium sulfate and concentrated to give N-methoxy-N-methyl-3-{[3-methoxy-4-(5-methyl-2-phenyl-1,3-oxazol-4-ylmethoxy)benzyl]oxy}-1-methyl-1H-pyrazole-4-carboxamide (3.63 g, yield 96%) as colorless crystals. The crystals were recrystallized from acetone-hexane. melting point: 138-139° C.

후처리

  1. stirringthe mixture was stirred overnight at room temperature
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe ethyl acetate layer was washed successively with dilute hydrochloric acid, saturated aqueous sodium hydrogen carbonate and saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-5b4f49ad74714244a183a1679457dd56
출처 데이터셋
uspto-grants-2008_05
특허 번호
US07368578B2

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