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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Sodium sulfate decahydrate → [4-(6-aminomethyl-1-methyl-1H-benzimidazol-2-yl)-benzyl]-dipropyl-amine

HRID 2080796
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인쇄 미리보기

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HRID 2080796 반응식
[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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran
용매
2회

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-74d36e780d684fe8b35c87cdbf385651
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07932281B2

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