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Hexane → 6-[2-n-Butyl-1-{(2-chlorophenyl)methyl}-1H-imidazol-5yl]-4-hexenoic acid

HRID 260751
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HRID 260751 반응식
[Br-].[C:2]([CH2:5][CH2:6][CH2:7][CH2:8][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)([OH:4])=[O:3].C([Li])CCC.CCCCCC.[CH2:39]([C:43]1[N:44]([CH2:50][C:51]2[CH:56]=[CH:55][CH:54]=[CH:53][C:52]=2[Cl:57])[C:45]([CH:48]=O)=[CH:46][N:47]=1)[CH2:40][CH2:41][CH3:42]>O1CCCC1.O>[CH2:39]([C:43]1[N:44]([CH2:50][C:51]2[CH:56]=[CH:55][CH:54]=[CH:53][C:52]=2[Cl:57])[C:45]([CH2:48][CH:8]=[CH:7][CH2:6][CH2:5][C:2]([OH:4])=[O:3])=[CH:46][N:47]=1)[CH2:40][CH2:41][CH3:42]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8058HexaneHCID 161236(4-Carboxybutyl)triphenylphosphonium bromideHCID 101075301H-Imidazole-5-carboxaldehyde, 2-butyl-1-[(2-chlorophenyl)methyl]-HCID 178418339Butyllithium

생성물 1

HCID 540265716-[2-n-Butyl-1-{(2-chlorophenyl)methyl}-1H-imidazol-5yl]-4-hexenoic acid수율 36.7%

시약·촉매·용매 2

HCID 962
Water
용매
HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
0 °C

실험 절차

To a suspension of (4-carboxybutyl)triphenyl-phosphonium bromide (1.04 g, 2.35 mmol) in dry tetrahydrofuran (25 mL) at 0° C. under argon was added n-butyl lithium in hexane (1.8 mL of 2.5M, 4.6 mmol). The reaction mixture was stirred for 15 minutes at 0° C. and then a solution of 2-n-butyl-1-(2-chlorophenyl)methyl-1H-imidazol-5-carboxaldehyde [Example 6 (iii)] (0.5 g, 1.81 mmol) in tetrahydrofuran (25 mL) was added dropwise. The mixture was stirred an additional hour at 0° C. and then at ambient temperature for 3 days. Water was added and the mixture was extracted with diethyl ether. The aqueous layer was acidified to pH 3 with aqueous hydrochloric acid solution. The product was extracted into ethyl acetate, washed with water, dried, concentrated, and chromatographed over silica gel eluting with 5-10% methanol in methylene chloride to give 0.24 g of 6-[2-n-butyl-1-{(2-chlorophenyl)methyl}-1H-imidazol-5-yl]-4-hexenoic acid.

후처리

  1. stirringThe mixture was stirred an additional hour at 0° C.
  2. waitat ambient temperature for 3 days
  3. extractionthe mixture was extracted with diethyl ether
  4. extractionThe product was extracted into ethyl acetate
  5. washwashed with water
  6. customdried
  7. concentrationconcentrated
  8. customchromatographed over silica gel eluting with 5-10% methanol in methylene chloride

출처 및 근거

ORD 기록
ord-f292aa281dd543869c402cc2b082136b
출처 데이터셋
uspto-grants-1996_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05530017

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