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Dicyclohexylcarbodiimide → 8-Fluoro-isoquinoline-3-carboxylic acid{(s)-1-azabicyclo[2.2.2]oct-2-yl}-amide

HRID 2245286
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HRID 2245286 반응식
C1([N:7]=[C:8]=[N:9][CH:10]2[CH2:15][CH2:14][CH2:13][CH2:12]C2)CCCCC1.[F:16][C:17]1[CH:18]=[CH:19][CH:20]=[C:21]2[C:26]=1[CH:25]=[N:24][C:23]([C:27]([OH:29])=O)=[CH:22]2.[CH2:30](N(C(C)C)C(C)C)C.OC1C2N=NNC=2C=CC=1.N12CCC(CC1)[C@H](N)C2>CN(C=O)C>[N:9]12[CH2:10][CH2:15][CH:14]([CH2:13][CH2:12]1)[CH2:30][C@H:8]2[NH:7][C:27]([C:23]1[N:24]=[CH:25][C:26]2[C:21]([CH:22]=1)=[CH:20][CH:19]=[CH:18][C:17]=2[F:16])=[O:29]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 10868DicyclohexylcarbodiimideHCID 81531Diisopropylethylamine2회HCID 719216(S)-quinuclidin-3-amineHCID 685453938-Fluoroisoquinoline-3-carboxylic acidHCID 178418300HCID 178418300, 화합물

생성물 1

HCID 685505888-Fluoro-isoquinoline-3-carboxylic acid{(s)-1-azabicyclo[2.2.2]oct-2-yl}-amide
수율 35%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Dicyclohexyl-carbodiimide (7.69 g, 30 mmol) is added to a solution of 8-fluoro-isoquinoline-3-carboxylic acid (5.1 g, 22.4 mmol), ethyl-diisopropyl-amine (4.6 ml, 26.88 mmol) and hydroxybenzotriazole (5.36 g, 33.6 mmol) in DMF (150 ml). The mixture is stirred for 2 hours at room temperature. (S)-(1-Aza-bicyclo[2.2.2]oct-3-yl)amine (4.46 g, 49.28 mmol) and ethyl-diisopropyl-amine (8.7 ml, 49.28 mmol) are added and the solution is stirred for another 18 hours at room temperature. The solvent is removed by evaporation and the residue is dissolved in methylenedichloride and washed with a saturated K2CO3 solution and brine. The organic layer is dried over MgSO4 and evaporated. The crude product is purified by chromatography (CH2Cl2/MeOH/NH4OH, 92.5/7.5/0.75) to afford the desired compound (2.35 g). The product is recrystallized from ethanolic HCl to give 2 g. of the hydrochloric salt.

후처리

  1. stirringthe solution is stirred for another 18 hours at room temperature
  2. customThe solvent is removed by evaporation
  3. dissolutionthe residue is dissolved in methylenedichloride
  4. washwashed with a saturated K2CO3 solution and brine
  5. dry with materialThe organic layer is dried over MgSO4
  6. customevaporated
  7. customThe crude product is purified by chromatography (CH2Cl2/MeOH/NH4OH, 92.5/7.5/0.75)

출처 및 근거

ORD 기록
ord-71871602fe904859a754ca0db7e542e5
출처 데이터셋
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07683075B2

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