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Diisopropylethylamine → HCID 178496555, 화합물

HRID 1260708
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HRID 1260708 반응식
CO[C:3](=[O:12])[CH2:4][C@H:5]1[CH2:9][CH2:8][C@H:7]([O:10][CH3:11])[CH2:6]1.O([Si](C)(C)C)[K].Cl.Cl.Cl.[S:22]1[C:26]2=[C:27]([N:31]3[CH2:36][CH2:35][N:34]([CH2:37][CH2:38][C@H:39]4[CH2:44][CH2:43][C@H:42]([NH2:45])[CH2:41][CH2:40]4)[CH2:33][CH2:32]3)[N:28]=[CH:29][CH:30]=[C:25]2[CH:24]=[CH:23]1.CCN(C(C)C)C(C)C.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.C([O-])(O)=O.[Na+]>C(Cl)Cl>[CH3:11][O:10][C@H:7]1[CH2:8][CH2:9][C@H:5]([CH2:4][C:3]([NH:45][C@H:42]2[CH2:43][CH2:44][C@H:39]([CH2:38][CH2:37][N:34]3[CH2:35][CH2:36][N:31]([C:27]4[N:28]=[CH:29][CH:30]=[C:25]5[CH:24]=[CH:23][S:22][C:26]=45)[CH2:32][CH2:33]3)[CH2:40][CH2:41]2)=[O:12])[CH2:6]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 6

HCID 81531DiisopropylethylamineHCID 516892Sodium BicarbonateHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 59598533Racemic trans-(3-methoxy-cyclopentyl)-acetic acid methyl esterHCID 178478591HCID 178478591, 화합물2회HCID 178504318HCID 178504318, 화합물

생성물

1
HCID 178496555HCID 178496555, 화합물수율 68%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of racemic trans-(3-methoxy-cyclopentyl)-acetic acid methyl ester [WO 2009/019174] (41 mg, 0.24 mmol) and KOSiMe3 (51 mg, 0.40 mmol) in CH2Cl2 (1 ml) was stirred at room temperature over night. The solvent was evaporated and DMF (1 ml) was added followed by trans-4-[2-(4-thieno[2,3-c]pyridin-7-yl-piperazin-1-yl)-ethyl]-cyclohexylamine trihydrochloride (intermediate A; 90 mg, 0.20 mmol), DIPEA (103 mg, 0.80 mmol) and TBTU (83 mg, 0.26 mmol). After stirring 3 h at room temperature, sat. aq. NaHCO3 sol. was added and the product was extracted with CH2Cl2. The organic layer was dried (MgSO4), the solvent was evaporated and the crude product was purified by flash chromatography on silica gel (CH2Cl2/MeOH 95:5) to yield the title compound as a light red foam (65 mg, 68%), MS (ISP) m/z=485.4 [(M+H)+].

후처리

  1. customThe solvent was evaporated
  2. additionDMF (1 ml) was added
  3. stirringAfter stirring 3 h at room temperature
  4. extractionthe product was extracted with CH2Cl2
  5. dry with materialThe organic layer was dried (MgSO4)
  6. customthe solvent was evaporated
  7. customthe crude product was purified by flash chromatography on silica gel (CH2Cl2/MeOH 95:5)

출처 및 근거

ORD 기록
ord-60bdb4b885c44507b3258f7a923d8004
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08470828B2

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