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Nitrogen → 5-[4-(1,1-Dioxidothiomorpholin-4-yl)phenyl]-2-({6-[(2-hydroxy-2-methylpropoxy)methyl]pyridin-2-yl}amino)thiophene-3-carboxamide

HRID 385853
ノート
印刷プレビュー

反応式

HRID 385853 の反応式
[O:1]=[S:2]1(=[O:25])[CH2:7][CH2:6][N:5]([C:8]2[CH:13]=[CH:12][C:11]([C:14]3[S:18][C:17]([N+:19]([O-])=O)=[C:16]([C:22]([NH2:24])=[O:23])[CH:15]=3)=[CH:10][CH:9]=2)[CH2:4][CH2:3]1.N#N.Br[C:29]1[N:34]=[C:33]([CH2:35][O:36][CH2:37][C:38]([CH3:41])([OH:40])[CH3:39])[CH:32]=[CH:31][CH:30]=1.CC(C1C=C(C(C)C)C(C2C=CC=CC=2P(C2CCCCC2)C2CCCCC2)=C(C(C)C)C=1)C.C([O-])([O-])=O.[K+].[K+]>CO.[Pt].C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[O:1]=[S:2]1(=[O:25])[CH2:7][CH2:6][N:5]([C:8]2[CH:13]=[CH:12][C:11]([C:14]3[S:18][C:17]([NH:19][C:29]4[CH:30]=[CH:31][CH:32]=[C:33]([CH2:35][O:36][CH2:37][C:38]([OH:40])([CH3:39])[CH3:41])[N:34]=4)=[C:16]([C:22]([NH2:24])=[O:23])[CH:15]=3)=[CH:10][CH:9]=2)[CH2:4][CH2:3]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 947NitrogenHCID 11430Potassium CarbonateHCID 111557942-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenylHCID 583352721-[(6-Bromopyridin-2-yl)methoxy]-2-methylpropan-2-olHCID 595262725-[4-(1,1-Dioxidothiomorpholin-4-yl)phenyl]-2-nitrothiophene-3-carboxamide2 回

生成物 1

HCID 59526138
5-[4-(1,1-Dioxidothiomorpholin-4-yl)phenyl]-2-({6-[(2-hydroxy-2-methylpropoxy)methyl]pyridin-2-yl}amino)thiophene-3-carboxamide

試薬・触媒・溶媒 3

HCID 23939Platinum触媒HCID 9811564Bis(dibenzylideneacetone)palladium触媒HCID 887Methanol溶媒

反応条件

温度
100 °C

実験手順

5-[4-(1,1-Dioxidothiomorpholin-4-yl)phenyl]-2-nitrothiophene-3-carboxamide (Intermediate 16) (525 mg, 1.376 mmol) and Pt/C, doped with V (90 mg, 0.014 mmol) were stirred at room temperature overnight in degassed MeOH (5 mL) under a balloon of H2. The vial was then evacuated and back-filled with N2 (4×) and 1-[(6-bromopyridin-2-yl)methoxy]-2-methylpropan-2-ol (Example 217 Step 1) (358 mg, 1.38 mmol), Pd2dba3 (126 mg, 0.138 mmol), X-Phos (328 mg, 0.69 mmol) and K2CO3 (209 mg, 1.51 mmol) were added. The vial was evacuated and back-filled with N2 (3×) and the resulting mixture was stirred at 100° C. for 4 hours. After cooling to room temperature, the mixture was diluted with methanol, silica gel was added, and the solvent was removed in vacuo. Purification of the residue by silica gel chromatography (0-6% MeOH—CHCl3) gave the title compound as a beige solid after triturating in DCM.

後処理

  1. customThe vial was then evacuated
  2. additionwere added
  3. customThe vial was evacuated
  4. additionback-filled with N2 (3×)
  5. temperatureAfter cooling to room temperature
  6. additionthe mixture was diluted with methanol, silica gel
  7. additionwas added
  8. customthe solvent was removed in vacuo
  9. customPurification of the residue by silica gel chromatography (0-6% MeOH—CHCl3)

出典と根拠

ORDレコード
ord-e9894cec37e1472cbce33b0fd2a35a29
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08367706B2

反応ノート

読み込み中…

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