Maleic Acid → HCID 68525872、化合物

HRID 1932547ノート

反応式

HRID 1932547 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:27]=[CH:28][C:29]=1[Cl:30])[C:5]([NH:7][C:8]1[CH:9]=[CH:10][C:11]([O:14][C:15]2C=CC(CNCC(O)=O)=[CH:17][CH:16]=2)=[N:12][CH:13]=1)=[O:6].[O:31]1[C:36]2[CH:37]=[CH:38][C:39]([CH2:41][N:42]3[CH2:47][CH2:46][NH:45][CH2:44][CH2:43]3)=[CH:40][C:35]=2[O:34][CH2:33][CH2:32]1.O.ON1C2C=CC=CC=2N=N1.Cl.C(N=C=N[CH2:65][CH2:66][CH2:67][N:68]([CH3:70])[CH3:69])C.[C:71]([OH:78])(=[O:77])/[CH:72]=[CH:73]\[C:74]([OH:76])=[O:75]>CN(C=O)C>[C:71]([OH:78])(=[O:77])/[CH:72]=[CH:73]\[C:74]([OH:76])=[O:75].[Cl:1][C:2]1[CH:3]=[C:4]([CH:27]=[CH:28][C:29]=1[Cl:30])[C:5]([NH:7][C:8]1[CH:13]=[N:12][C:11]([O:14][C:15]2[CH:65]=[CH:66][C:67]([N:68]([CH2:69][C:74]([N:45]3[CH2:46][CH2:47][N:42]([CH2:41][C:39]4[CH:38]=[CH:37][C:36]5[O:31][CH2:32][CH2:33][O:34][C:35]=5[CH:40]=4)[CH2:43][CH2:44]3)=[O:75])[CH3:70])=[CH:17][CH:16]=2)=[CH:10][CH:9]=1)=[O:6]

参加物

7

反応物 5

HCID 444266Maleic AcidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 49622611-[(2,3-Dihydro-1,4-benzodioxin-6-yl)methyl]piperazineHCID 68525947HCID 68525947、化合物

生成物 1

HCID 68525872HCID 68525872、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of ({4-[5-(3,4-dichlorobenzoyl-amino)pyridin-2-yloxy]phenyl}methylamino)acetic acid (2.50 g, 5.6 mmol) in DMF (55 mL) were added 1-(2,3-dihydrobenzo[1,4]dioxin-6-ylmethyl)piperazine (1.7 g, 7.3 mmol), 1-hydroxybenzotriazole monohydrate (0.86 g, 5.6 mmol) and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (1.29 g, 6.7 mmol) under ice cooling, and the resulting solution was stirred for 30 minutes under ice cooling and for 17 hours at room temperature. This reaction solution was concentrated under reduced pressure. Water was added to the residue, and extracted with ethyl acetate. The ethyl acetate layer was washed with a saturated sodium bicarbonate solution and brine, dried over anhydrous magnesium sulfate, and evaporated. The residue was dissolved in ethanol (30 mL). To the resulting solution was added maleic acid (0.32 g, 2.7 mmol), and this solution was left to stand. The precipitates were collected by filtration, to thereby yield 1.45 g of the title compound.

後処理

  1. concentrationThis reaction solution was concentrated under reduced pressure
  2. additionWater was added to the residue
  3. extractionextracted with ethyl acetate
  4. washThe ethyl acetate layer was washed with a saturated sodium bicarbonate solution and brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customevaporated
  7. dissolutionThe residue was dissolved in ethanol (30 mL)
  8. waitthis solution was left
  9. filtrationThe precipitates were collected by filtration

出典と根拠

ORDレコード
ord-6e311abed25b4fec870e30460af4a165
出典データセット
uspto-grants-2012_05
特許番号
US08188277B2

反応ノート

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