Toluene → HCID 70044288, 화합물

HRID 1646125노트

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HRID 1646125 반응식
[CH2:1]([C:5]1[N:6]([CH2:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=2[Cl:30])[C:7](/[CH:10]=[C:11](\[CH2:16][C:17]2[O:18][C:19]([CH3:22])=[CH:20][CH:21]=2)/[C:12](OC)=[O:13])=[CH:8][N:9]=1)[CH2:2][CH2:3][CH3:4].[H-].C([Al+]CC(C)C)C(C)C.C1(C)C=CC=CC=1>O1CCCC1>[CH2:1]([C:5]1[N:6]([CH2:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=2[Cl:30])[C:7](/[CH:10]=[C:11](\[CH2:16][C:17]2[O:18][C:19]([CH3:22])=[CH:20][CH:21]=2)/[CH2:12][OH:13])=[CH:8][N:9]=1)[CH2:2][CH2:3][CH3:4]

참가 물질

5

반응물 3

HCID 1140TolueneHCID 21225700DiisobutylaluminumhydrideHCID 86746470methyl (E)-3-[2-n-butyl-1-{(2-chlorophenyl)methyl}-1H-imidazol-5-yl]-2-(5-methyl-2-furyl)methyl-2-propenoate

생성물 1

HCID 70044288HCID 70044288, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of methyl (E)-3-[2-n-butyl-1-{(2-chlorophenyl)methyl}-1H-imidazol-5-yl]-2-(5-methyl-2-furyl)methyl-2-propenoate (Example 6, Method A) (1.5 mmol) in dry tetrahydrofuran (10 mL) held at -78° C. under argon is treated dropwise with a solution of diisobutyl aluminum hydride in toluene (3.30 mmol, 2.2 mL of 1.5M). The mixture is allowed to warm to ambient temperature and stirred an additional 17 hours. Excess reducing agent is quenched with methanol and water, dilute acetic acid and methylene dichloride are added, and the organic layer is washed with sodium bicarbonate solution, dried and concentrated to give the title compound.

후처리

  1. customheld at -78° C. under argon
  2. customis quenched with methanol and water, dilute acetic acid and methylene dichloride
  3. additionare added
  4. washthe organic layer is washed with sodium bicarbonate solution
  5. customdried
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-3ced3df609d3443e92f904ee61d7f58d
출처 데이터셋
uspto-grants-1993_01
특허 번호
US05177096

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