Aluminium lithium hydride → HCID 69075874, 화합물

HRID 2110024노트

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HRID 2110024 반응식
C[O:2][C:3]([C:5]1[CH:48]=[CH:47][C:8]2[N:9]([CH2:39][O:40][CH2:41][CH2:42][Si:43]([CH3:46])([CH3:45])[CH3:44])[C:10]([N:12]([CH2:21][CH:22]3[CH2:27][CH2:26][N:25]([CH2:28][C:29]4[C:38]5[C:33](=[CH:34][CH:35]=[CH:36][CH:37]=5)[CH:32]=[CH:31][CH:30]=4)[CH2:24][CH2:23]3)[CH2:13][O:14][CH2:15][CH2:16][Si:17]([CH3:20])([CH3:19])[CH3:18])=[N:11][C:7]=2[CH:6]=1)=O.[H-].[Li+].[Al+3].[H-].[H-].[H-]>O1CCCC1>[C:29]1([CH2:28][N:25]2[CH2:24][CH2:23][CH:22]([CH2:21][N:12]([CH2:13][O:14][CH2:15][CH2:16][Si:17]([CH3:20])([CH3:19])[CH3:18])[C:10]3[N:9]([CH2:39][O:40][CH2:41][CH2:42][Si:43]([CH3:44])([CH3:45])[CH3:46])[C:8]4[CH:47]=[CH:48][C:5]([CH2:3][OH:2])=[CH:6][C:7]=4[N:11]=3)[CH2:27][CH2:26]2)[C:38]2[C:33](=[CH:34][CH:35]=[CH:36][CH:37]=2)[CH:32]=[CH:31][CH:30]=1

참가 물질

4

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 690756512-[(1-naphthalen-1-ylmethyl-piperidin-4-ylmethyl)-(2-trimethylsilanyl-ethoxymethyl)-amino]-1-(2-trimethylsilanyl-ethoxymethyl)-1H-benzimidazole-5-carboxylic acid methyl ester

생성물 1

HCID 69075874HCID 69075874, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

After dissolving 2-[(1-naphthalen-1-ylmethyl-piperidin-4-ylmethyl)-(2-trimethylsilanyl-ethoxymethyl)-amino]-1-(2-trimethylsilanyl-ethoxymethyl)-1H-benzimidazole-5-carboxylic acid methyl ester (624 mg, 0.91 mmol) in anhydrous tetrahydrofuran (10 ml) under a nitrogen stream, aluminum lithium hydride (72.4 mg, 1.82 mmol) was added at 0° C., and the mixture was stirred for 2 hours. After then adding a saturated aqueous sodium sulfate solution, extraction was performed with ethyl acetate and then with dichloromethane. Each extract was washed with saturated brine, and then combined and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain [2-[(1-naphthalen-1-ylmethyl-piperidin -4-ylmethyl)-(2-trimethylsilanyl-ethoxymethyl)-amino]-1-(2-trimethylsilanyl-ethoxymethyl)-1H-benzimidazol-5-yl]-methanol. The compound was identified by LC-MS.

후처리

  1. additionwas added at 0° C.
  2. additionAfter then adding
  3. extractiona saturated aqueous sodium sulfate solution, extraction
  4. washEach extract was washed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationThe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-60f78bdc023c4cc49ed65e3a39cefacf
출처 데이터셋
uspto-grants-2009_04
특허 번호
US07517875B2

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