Sodium sulfate decahydrate → [2-(4-dipropylaminobutyl)-3-propyl-3H-benzimidazol-5-yl]methanol

HRID 1174010노트

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HRID 1174010 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].C[O:8][C:9]([C:11]1[CH:33]=[CH:32][C:14]2[N:15]=[C:16]([CH2:21][CH2:22][CH2:23][CH2:24][N:25]([CH2:29][CH2:30][CH3:31])[CH2:26][CH2:27][CH3:28])[N:17]([CH2:18][CH2:19][CH3:20])[C:13]=2[CH:12]=1)=O.O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[CH2:29]([N:25]([CH2:26][CH2:27][CH3:28])[CH2:24][CH2:23][CH2:22][CH2:21][C:16]1[N:17]([CH2:18][CH2:19][CH3:20])[C:13]2[CH:12]=[C:11]([CH2:9][OH:8])[CH:33]=[CH:32][C:14]=2[N:15]=1)[CH2:30][CH3:31]

참가 물질

5

반응물 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 669418292-(4-dipropylaminobutyl)-3-propyl-3H-benzimidazole-5-carboxylic Acid Methyl Ester

생성물 1

HCID 23079221[2-(4-dipropylaminobutyl)-3-propyl-3H-benzimidazol-5-yl]methanol수율 90.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
0 °C

실험 절차

Lithium aluminum hydride (138 mg) was suspended in THF (7 ml) and then cooled to 0° C. After that, a solution of the compound (361 mg) obtained in Example 125-3 in THF (7 ml) was dropped in the suspension, followed by stirring at 0° C. for 1 hour. After completion of the reaction, sodium sulfate decahydrate was continuously added to the solution until bubbling was stopped, and a 1 mol/l sodium hydroxide aqueous solution was then added to the mixture until a white precipitate was generated. Solid matter was separated through filtration and the solvent was then distilled off from the filtrate under reduced pressure. The residue was dried under vacuum, thereby obtaining the subject compound (302 mg) as a pale-yellow viscous substance.

후처리

  1. additionwas continuously added to the solution
  2. customuntil bubbling
  3. additiona 1 mol/l sodium hydroxide aqueous solution was then added to the mixture until a white precipitate
  4. customSolid matter was separated through filtration
  5. distillationthe solvent was then distilled off from the filtrate under reduced pressure
  6. customThe residue was dried under vacuum

출처 및 근거

ORD 기록
ord-156f4c780fb34e46ad1b39226f64e3ea
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07833991B2

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