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Tetrahydrofuran → HCID 18545432、化合物

HRID 564867
ノート
印刷プレビュー

反応式

HRID 564867 の反応式
C1C[O:4][CH2:3]C1.Cl[C:7]1[N:12]=[C:11]([N:13]2[C:17]([CH3:18])=[C:16](/[CH:19]=[CH:20]/[CH2:21][N:22]3[CH2:27][CH2:26][N:25]([C:28]4[CH:33]=[C:32]([F:34])[CH:31]=[C:30]([F:35])[CH:29]=4)[CH2:24][CH2:23]3)[CH:15]=[N:14]2)[CH:10]=[C:9]([CH3:36])[N:8]=1.CO[C:39]1[CH:46]=[CH:45][C:42]([CH2:43][NH2:44])=[CH:41][CH:40]=1.C(=O)([O-])[O-].[K+].[K+]>C(Cl)(Cl)Cl>[F:35][C:30]1[CH:29]=[C:28]([N:25]2[CH2:26][CH2:27][N:22]([CH2:21]/[CH:20]=[CH:19]/[C:16]3[CH:15]=[N:14][N:13]([C:11]4[CH:10]=[C:9]([CH3:36])[N:8]=[C:7]([NH:44][CH2:43][C:42]5[CH:41]=[CH:40][CH:39]=[CH:46][C:45]=5[O:4][CH3:3])[N:12]=4)[C:17]=3[CH3:18])[CH2:23][CH2:24]2)[CH:33]=[C:32]([F:34])[CH:31]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8028TetrahydrofuranHCID 11430Potassium CarbonateHCID 754524-MethoxybenzylamineHCID 18545346HCID 18545346、化合物

生成物 1

HCID 18545432HCID 18545432、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To 15 ml of a THF solution of 155 mg of the compound obtained in Example 35 were added 240 mg of p-methoxybenzylamine and 50 mg (0.362 mmol) of potassium carbonate, followed by refluxing for 60 hours. Chloroform was added to the reaction mixture, and the mixture was washed with a saturated sodium chloride aqueous solution. The combined organic layer was dried over anhydrous sodium sulfate, and the solvent was evaporated. The residue was subjected to silica gel column chromatography using a 99:1 mixture (by volume) of chloroform and methanol as a developing solution. The fraction containing the desired compound was concentrated to give 183 mg of the title compound.

後処理

  1. temperatureby refluxing for 60 hours
  2. washthe mixture was washed with a saturated sodium chloride aqueous solution
  3. dry with materialThe combined organic layer was dried over anhydrous sodium sulfate
  4. customthe solvent was evaporated
  5. additionThe fraction containing the desired compound
  6. concentrationwas concentrated

出典と根拠

ORDレコード
ord-98920d4eb731462887356aeca375528a
出典データセット
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06169086A

反応ノート

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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