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Diisopropylethylamine → HCID 178496556、化合物

HRID 2042411
ノート
印刷プレビュー

反応式

HRID 2042411 の反応式
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.[O:22]1[C:30]2[CH:29]=[CH:28][N:27]=[C:26]([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)[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>[O:22]1[C:30]2[CH:29]=[CH:28][N:27]=[C:26]([N:31]3[CH2:36][CH2:35][N:34]([CH2:37][CH2:38][C@H:39]4[CH2:44][CH2:43][C@H:42]([NH:45][C:3](=[O:12])[CH2:4][C@H:5]5[CH2:9][CH2:8][C@H:7]([O:10][CH3:11])[CH2:6]5)[CH2:41][CH2:40]4)[CH2:33][CH2:32]3)[C:25]=2[CH:24]=[CH:23]1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 6

HCID 81531DiisopropylethylamineHCID 516892Sodium BicarbonateHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 59598533Racemic trans-(3-methoxy-cyclopentyl)-acetic acid methyl esterHCID 178478592HCID 178478592、化合物2 回HCID 178504318HCID 178504318、化合物

生成物

1
HCID 178496556HCID 178496556、化合物収率 78.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of racemic trans-(3-methoxy-cyclopentyl)-acetic acid methyl ester [WO 2009/019174] (70 mg, 0.41 mmol) and KOSiMe3 (88 mg, 0.69 mmol) in CH2Cl2 (1.5 ml) was stirred at room temperature over night. The solvent was evaporated and DMF (1.5 ml) was added followed by trans-4-[2-(4-furo[3,2-c]pyridin-4-yl-piperazin-1-yl)-ethyl]-cyclohexylamine trihydrochloride (intermediate A) (150 mg, 0.34 mmol), DIPEA (177 mg, 1.37 mmol) and TBTU (143 mg, 0.44 mmol). After stirring 4 h at room temperature, sat. aq. NaHCO3 sol. was added and the product was extracted with CH2Cl2. The organic layer was dried (Na2SO4), the solvent was evaporated and the crude product was purified by flash chromatography on silica gel (CH2Cl2/MeOH/25% NH3 aq 140:10:1) to yield the title compound as a white solid (125 mg, 78%), MS (ISP) m/z=469.3 [(M+H)+].

後処理

  1. customThe solvent was evaporated
  2. additionDMF (1.5 ml) was added
  3. stirringAfter stirring 4 h at room temperature
  4. extractionthe product was extracted with CH2Cl2
  5. dry with materialThe organic layer was dried (Na2SO4)
  6. customthe solvent was evaporated
  7. customthe crude product was purified by flash chromatography on silica gel (CH2Cl2/MeOH/25% NH3 aq 140:10:1)

出典と根拠

ORDレコード
ord-55e76aa2526440e1b2b10e0f032d7df8
出典データセット
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08586579B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート