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

HRID 2080716노트

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HRID 2080716 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 (7.0 ml) and then the whole was cooled to 0° C. After that, a THF solution (7.0 ml) containing the compound (361 mg) obtained in Example 3-3 was dropped in the suspension, followed by stirring at 0° C. for 1 hour. After completion of the reaction, sodium sulfate decahydrate was 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. The solid component 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 oily substance.

후처리

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

출처 및 근거

ORD 기록
ord-51b4d309d753401a9995646e80da9717
출처 데이터셋
uspto-grants-2011_04
특허 번호
US07932281B2

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