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Water → [4-[2-(4-Dibutylamino-2-methoxyphenyl)vinyl]phenyl]methanol

HRID 85249
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HRID 85249 반응식
[CH2:1]([N:5]([CH2:41][CH2:42][CH2:43][CH3:44])[C:6]1[CH:11]=[CH:10][C:9]([CH:12]=[CH:13][C:14]2[CH:19]=[CH:18][C:17]([CH2:20][O:21][Si](C(C)(C)C)(C3C=CC=CC=3)C3C=CC=CC=3)=[CH:16][CH:15]=2)=[C:8]([O:39][CH3:40])[CH:7]=1)[CH2:2][CH2:3][CH3:4].[F-].C([N+](CCCC)(CCCC)CCCC)CCC.O.C(OCC)(=O)C>O1CCCC1>[CH2:41]([N:5]([CH2:1][CH2:2][CH2:3][CH3:4])[C:6]1[CH:11]=[CH:10][C:9]([CH:12]=[CH:13][C:14]2[CH:15]=[CH:16][C:17]([CH2:20][OH:21])=[CH:18][CH:19]=2)=[C:8]([O:39][CH3:40])[CH:7]=1)[CH2:42][CH2:43][CH3:44]
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참가 물질

6

반응물 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 2724141Tetrabutylammonium FluorideHCID 68008966Dibutyl[4-[2-[4-(tert-butyldiphenylsiloxymethyl)phenyl]vinyl]-3-methoxyphenyl]amine

생성물 1

HCID 68009291[4-[2-(4-Dibutylamino-2-methoxyphenyl)vinyl]phenyl]methanol수율 96.4%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

실험 절차

In 50 ml of tetrahydrofuran was dissolved 3.9 g (6.44 mmol) of dibutyl[4-[2-[4-(tert-butyldiphenylsiloxymethyl)phenyl]vinyl]-3-methoxyphenyl]amine, and 20 ml of tetrabutylammonium fluoride (1 mol solution in tetrahydrofuran) was added dropwise thereto with stirring at room temperature. The mixture was stirred for 2.5 hours. After the reaction mixture was poured into water, extraction with ethyl acetate, washing with a saturated saline solution, drying over anhydrous sodium sulfate, and concentration were performed. The residue was purified by silica gel column chromatography to give 2.28 g of a yellow liquid (yield: 96.4%).

후처리

  1. additionwas added dropwise
  2. stirringThe mixture was stirred for 2.5 hours
  3. washwashing with a saturated saline solution
  4. dry with materialdrying over anhydrous sodium sulfate, and concentration
  5. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-923aeb04d36d41329445702d905d360c
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08846955B2

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