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1-Phenylpiperazine → HCID 18348553, 화합물

HRID 2268535
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HRID 2268535 반응식
[CH3:1][O:2][C:3]1[C:4](=[O:29])[C:5]2[CH2:6][CH:7]([CH2:15][CH2:16][CH2:17][CH2:18][O:19][C:20]3[CH:28]=[CH:27][C:23]([C:24](O)=[O:25])=[CH:22][CH:21]=3)[CH2:8][C:9]=2[C:10](=[O:14])[C:11]=1[O:12][CH3:13].[C:30]1(N2CCNCC2)[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1.Cl.C(N=C=NCCCN(C)C)C.O.O[N:56]1[C:60]2C=[CH:62][CH:63]=[CH:64][C:59]=2N=N1>C1COCC1.O.C(N(CC)CC)C>[CH3:1][O:2][C:3]1[C:4](=[O:29])[C:5]2[CH2:6][CH:7]([CH2:15][CH2:16][CH2:17][CH2:18][O:19][C:20]3[CH:21]=[CH:22][C:23]([C:24]([N:56]4[CH2:62][CH2:63][CH:64]([C:30]5[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=5)[CH2:59][CH2:60]4)=[O:25])=[CH:27][CH:28]=3)[CH2:8][C:9]=2[C:10](=[O:14])[C:11]=1[O:12][CH3:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 70961-PhenylpiperazineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 18348629HCID 18348629, 화합물

생성물 1

HCID 18348553HCID 18348553, 화합물수율 58.9%

시약·촉매·용매 3

HCID 962
Water
용매
HCID 8028Tetrahydrofuran용매
HCID 8471Triethylamine용매

실험 절차

A mixture of 4-[4-(5,6-dimethoxy-4,7-dioxoindan-2-yl)butoxy]benzoic acid (500 mg), 1-phenylpiperazine (406 mg), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (479 mg), 1-hydroxybenzotriazole monohydrate (383 mg), triethylamine (0.697 ml) in THF (20 ml) was stirred at room temperature for 6 hr. The reaction mixture was diluted with water and extracted with combined solvent of THF and ethyl acetate. The organic layer was washed with water and saturated aqueous sodium chloride and dried. The solvent was removed in vacuo. The residue was recrystallized from THF-diisopropylether to yield the entitled compound (400 mg) as crystals.

후처리

  1. extractionextracted with combined solvent of THF and ethyl acetate
  2. washThe organic layer was washed with water and saturated aqueous sodium chloride
  3. customdried
  4. customThe solvent was removed in vacuo
  5. customThe residue was recrystallized from THF-diisopropylether

출처 및 근거

ORD 기록
ord-1a98a45a259744c5a26df9193208d99a
출처 데이터셋
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06326369B1

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