Morpholine → HCID 57901687, 화합물

HRID 1851547노트

반응식

HRID 1851547 반응식
[CH3:1][N:2]([S:22]([C:25]1[S:26][CH:27]=[CH:28][CH:29]=1)(=[O:24])=[O:23])[C:3]1[CH:4]=[CH:5][CH:6]=[C:7]2[C:11]=1[NH:10][C:9]([C:12]1[S:13][C:14]([CH2:17][CH2:18][C:19]([OH:21])=O)=[CH:15][N:16]=1)=[CH:8]2.N1(O)C2C=CC=CC=2N=N1.Cl.CN(C)CCCN=C=NCC.[NH:52]1[CH2:57][CH2:56][O:55][CH2:54][CH2:53]1>O.CN(C)C=O>[CH3:1][N:2]([C:3]1[CH:4]=[CH:5][CH:6]=[C:7]2[C:11]=1[NH:10][C:9]([C:12]1[S:13][C:14]([CH2:17][CH2:18][C:19]([N:52]3[CH2:57][CH2:56][O:55][CH2:54][CH2:53]3)=[O:21])=[CH:15][N:16]=1)=[CH:8]2)[S:22]([C:25]1[S:26][CH:27]=[CH:28][CH:29]=1)(=[O:23])=[O:24]

참가 물질

7

반응물 4

HCID 8083MorpholineHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 57901696HCID 57901696, 화합물

생성물 1

HCID 57901687HCID 57901687, 화합물수율 69.3%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

To a mixture of 3-(2-{7-[methyl(2-thienylsulfonyl)amino]-1H-indol-2-yl}-1,3-thiazol-5-yl)propanoic acid (0.30 g), 1H-1,2,3-benzotriazol-1-ol (0.11 g) and N,N-dimethylformamide (8 mL) was added N-[3-(dimethylamino)propyl]-N′-ethylcarbodiimide hydrochloride (0.15 g) at room temperature. The mixture was stirred at room temperature for 2 hr, and morpholine (0.30 g) was added. The reaction mixture was stirred at room temperature overnight, and water was added. The resulting crystals were collected by filtration and dried. The obtained crystals were subjected to silica gel column chromatography and the title compound (0.24 g, yield 69%) was obtained as yellow crystals from a fraction eluted with tetrahydrofuran-hexane (2:1, volume ratio). The crystals were recrystallized from ethyl acetate-hexane. melting point 160-161° C.

후처리

  1. stirringThe reaction mixture was stirred at room temperature overnight
  2. filtrationThe resulting crystals were collected by filtration
  3. customdried

출처 및 근거

ORD 기록
ord-7b0b0de4bd0e4f96bb7b0a9da9074c0e
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08957070B2

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