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Succinic Acid → 7-Chloro-6-[2-(cyclopropylmethyl-amino)-thiazol-5-ylthiomethyl]-2,3,4,5-tetrahydro-1H-benzo[d]azepine Succinate

HRID 1670569
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HRID 1670569 반응식
[Cl:1][C:2]1[CH:12]=[CH:11][C:5]2[CH2:6][CH2:7][NH:8][CH2:9][CH2:10][C:4]=2[C:3]=1[CH2:13][S:14][C:15]1[S:19][C:18]([NH:20][CH2:21][CH:22]2[CH2:24][CH2:23]2)=[N:17][CH:16]=1.[C:25]([OH:32])(=[O:31])[CH2:26][CH2:27][C:28]([OH:30])=[O:29]>C(O)C>[C:25]([OH:32])(=[O:31])[CH2:26][CH2:27][C:28]([OH:30])=[O:29].[Cl:1][C:2]1[CH:12]=[CH:11][C:5]2[CH2:6][CH2:7][NH:8][CH2:9][CH2:10][C:4]=2[C:3]=1[CH2:13][S:14][C:15]1[S:19][C:18]([NH:20][CH2:21][CH:22]2[CH2:24][CH2:23]2)=[N:17][CH:16]=1
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참가 물질

4

반응물 2

HCID 1110Succinic AcidHCID 598222607-chloro-6-[2-(cyclopropylmethyl-amino)-thiazol-5-ylthiomethyl]-2,3,4,5-tetrahydro-1H-benzo[d]azepine

생성물 1

HCID 866237077-Chloro-6-[2-(cyclopropylmethyl-amino)-thiazol-5-ylthiomethyl]-2,3,4,5-tetrahydro-1H-benzo[d]azepine Succinate수율 100.4%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 7-chloro-6-[2-(cyclopropylmethyl-amino)-thiazol-5-ylthiomethyl]-2,3,4,5-tetrahydro-1H-benzo[d]azepine (0.055 g, 0.144 mmol) in absolute ethanol (5 mL) add succinic acid (0.017 g, 0.144 mmol). After acid dissolves, concentrate the reaction mixture in vacuo. Combine the residue with MTBE, concentrate in vacuo several times and dry under high vacuum at room temperature overnight to obtain the title compound (0.072 g, 100%) as a white foam. MS (ES+) m/z: 380.0 (M+H)+.

후처리

  1. concentrationAfter acid dissolves, concentrate the reaction mixture in vacuo
  2. concentrationconcentrate in vacuo several times
  3. customdry under high vacuum at room temperature overnight

출처 및 근거

ORD 기록
ord-3d0a92f055d748a09f0ee0e730e27f26
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07994163B2

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