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Sodium sulfate decahydrate → [4-(6-aminomethyl-1-methyl-1H-benzimidazol-2-yl)-benzyl]-dipropyl-amine

HRID 2080796
ノート
印刷プレビュー

反応式

HRID 2080796 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([N:10]([CH2:14][C:15]1[CH:20]=[CH:19][C:18]([C:21]2[N:22]([CH3:32])[C:23]3[CH:29]=[C:28]([C:30]#[N:31])[CH:27]=[CH:26][C:24]=3[N:25]=2)=[CH:17][CH:16]=1)[CH2:11][CH2:12][CH3:13])[CH2:8][CH3:9].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[NH2:31][CH2:30][C:28]1[CH:27]=[CH:26][C:24]2[N:25]=[C:21]([C:18]3[CH:19]=[CH:20][C:15]([CH2:14][N:10]([CH2:7][CH2:8][CH3:9])[CH2:11][CH2:12][CH3:13])=[CH:16][CH:17]=3)[N:22]([CH3:32])[C:23]=2[CH:29]=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

5

反応物 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 231553902-(4-dipropylaminomethyl-phenyl)-3-methyl-3H-benzimidazol-5-carbonitrile

生成物 1

HCID 23155373[4-(6-aminomethyl-1-methyl-1H-benzimidazol-2-yl)-benzyl]-dipropyl-amine収率 59.6%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran
溶媒
2 回

反応条件

温度
0 °C

実験手順

Lithium aluminum hydride (64.0 mg) was suspended in THF (5.0 ml) and the whole was cooled to 0° C. A THF solution (5.0 ml) containing the compound (155 mg) obtained in Example 29-5 was dropped therein and the whole was stirred at 0° C. for 1 hour. After completion of the reaction, sodium sulfate decahydrate was added thereto until bubbling was stopped, and a 1 mol/l sodium hydroxide aqueous solution was then added thereto until a white precipitate was generated. A solid was separated by filtration and the solvent in the filtrate was then distillated off under reduced pressure, and the residue was dried under vacuum, thereby obtaining the subject compound (93.5 mg) as a yellow oily substance.

後処理

  1. additionwas dropped
  2. additionwas added
  3. customuntil bubbling
  4. additiona 1 mol/l sodium hydroxide aqueous solution was then added
  5. customA solid was separated by filtration
  6. customthe residue was dried under vacuum

出典と根拠

ORDレコード
ord-74d36e780d684fe8b35c87cdbf385651
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07932281B2

反応ノート

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