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HCID 14497520, 화합물 → HCID 14497596, 화합물

HRID 373488
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HRID 373488 반응식
[CH3:1][Mg]Br.[Cl:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[N:15]([C:16]3[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][CH:17]=3)[N:14]=[C:13]([CH2:24][CH2:25][CH:26]=[O:27])[CH:12]=2)=[CH:7][CH:6]=1>CCOCC>[Cl:4][C:5]1[CH:6]=[CH:7][C:8]([C:11]2[N:15]([C:16]3[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][CH:17]=3)[N:14]=[C:13]([CH2:24][CH2:25][CH:26]([OH:27])[CH3:1])[CH:12]=2)=[CH:9][CH:10]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14497520HCID 14497520, 화합물HCID 178418573HCID 178418573, 화합물

생성물 1

HCID 14497596HCID 14497596, 화합물수율 79%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

To a solution of methyl magnesium bromide (MeMgBr) (2.20 ml, 7.04 mM) in Et2O (15 ml) at 0° C. was added a solution of the aldehyde 11 (1.60 g, 4.69 mM)in Et2O (70 ml) dropwise over a 30 minute period. After stirring for 1 hour the reaction was quenched with a saturated, aqueous NH4Cl solution. The reaction mixture was partitioned between EtOAc and H2O. The EtOAc solution was dried (MgSO4), filtered, and concentrated in vacuo. Chromatography (65 g, Baker 40 gm silica gel) of the residue with Et2O as eluent afforded 20 (1.33 g, 79%) as a clear light yellow oil.

후처리

  1. customwas quenched with a saturated, aqueous NH4Cl solution
  2. customThe reaction mixture was partitioned between EtOAc and H2O
  3. dry with materialThe EtOAc solution was dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-4455a9c717254d299d340cf36d4c3116
출처 데이터셋
uspto-grants-1992_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05164381

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