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

HRID 2245286
ノート
印刷プレビュー

反応式

HRID 2245286 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 10868DicyclohexylcarbodiimideHCID 81531Diisopropylethylamine2 回HCID 719216(S)-quinuclidin-3-amineHCID 685453938-Fluoroisoquinoline-3-carboxylic acidHCID 178418300HCID 178418300、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-71871602fe904859a754ca0db7e542e5
出典データセット
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07683075B2

反応ノート

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