Potassium Sodium Tartrate → HCID 68989883、化合物

HRID 69483ノート

反応式

HRID 69483 の反応式
C[Al](C)C.[O:5]1[C:9]2([CH2:13][CH2:12][N:11]([C:14]3[CH:19]=[CH:18][C:17]([NH2:20])=[CH:16][C:15]=3[F:21])[CH2:10]2)[O:8][CH2:7][CH2:6]1.[CH3:22][O:23][C:24]1[CH:25]=[C:26]2[C:31](=[CH:32][CH:33]=1)[C:30](=[O:34])[O:29][CH2:28][CH2:27]2.[C@H](O)(C([O-])=O)[C@@H](O)C([O-])=O.[Na+].[K+]>C1(C)C=CC=CC=1.C(Cl)Cl>[O:8]1[C:9]2([CH2:13][CH2:12][N:11]([C:14]3[CH:19]=[CH:18][C:17]([NH:20][C:30](=[O:34])[C:31]4[CH:32]=[CH:33][C:24]([O:23][CH3:22])=[CH:25][C:26]=4[CH2:27][CH2:28][OH:29])=[CH:16][C:15]=3[F:21])[CH2:10]2)[O:5][CH2:6][CH2:7]1

参加物

7

反応物 4

HCID 9357Potassium Sodium TartrateHCID 124011826-Methoxy-3,4-dihydro-1H-2-benzopyran-1-oneHCID 16682925TrimethylaluminumHCID 211054314-(1,4-Dioxa-7-azaspiro[4.4]non-7-yl)-3-fluorophenylamine

生成物 1

HCID 68989883HCID 68989883、化合物

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

A 2M solution of trimethylaluminum in toluene (14.9 mL) was added dropwise at 0° C. to a solution of 4-(1,4-dioxa-7-aza-spiro[4.4]non-7-yl)-3-fluorophenylamine (5.3 g) in methylene chloride (100.8 mL). The reaction mixture was stirred for 15 min at 0° C. and then for 30 min at room temperature. Then a solution of 6-methoxy-isochroman-1-one (3.8 g) in methylene chloride (40 mL) was added dropwise. The reaction mixture was stirred overnight at room temperature. Then saturated Rochelle salt solution was carefully added and the mixture was stirred for 1 h at room temperature. The aqueous phase was extracted several times with methylene chloride. The organic phases were combined, dried over sodium sulfate and the solvent was removed in vacuum. In this way the product was obtained with molecular weight 416.17 (C22H25FN2O5); MS (ESI): 417 (M+H+).

後処理

  1. waitfor 30 min at room temperature
  2. stirringThe reaction mixture was stirred overnight at room temperature
  3. stirringthe mixture was stirred for 1 h at room temperature
  4. extractionThe aqueous phase was extracted several times with methylene chloride
  5. dry with materialdried over sodium sulfate
  6. customthe solvent was removed in vacuum
  7. customIn this way the product was obtained with molecular weight 416.17 (C22H25FN2O5)

出典と根拠

ORDレコード
ord-a97c7772dc6149feb9d3501c939816d1
出典データセット
uspto-grants-2014_09
特許番号
US08822495B2

反応ノート

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