1,2-Dichloroethane → HCID 66571158, 화합물

HRID 83614

반응식

HRID 83614 반응식
[Cl:1][C:2]1[CH:24]=[CH:23][C:5]([CH2:6][N:7]2[CH:11]=[CH:10][CH:9]=[C:8]2[C:12]([N:14]2[CH2:19][CH2:18][CH:17]([C:20]([OH:22])=O)[CH2:16][CH2:15]2)=[O:13])=[CH:4][CH:3]=1.CCN(C(C)C)C(C)C.C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1.[CH2:48]([NH2:55])[C:49]1[CH:54]=[CH:53][CH:52]=[CH:51][CH:50]=1>CN(C=O)C.CCOCC.CCOC(C)=O>[CH2:48]([NH:55][C:20]([CH:17]1[CH2:18][CH2:19][N:14]([C:12]([C:8]2[N:7]([CH2:6][C:5]3[CH:23]=[CH:24][C:2]([Cl:1])=[CH:3][CH:4]=3)[CH:11]=[CH:10][CH:9]=2)=[O:13])[CH2:15][CH2:16]1)=[O:22])[C:49]1[CH:54]=[CH:53][CH:52]=[CH:51][CH:50]=1

참가 물질

9

반응물 5

HCID 111,2-DichloroethaneHCID 7504BenzylamineHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 683802051-(1-(4-chlorobenzyl)-1H-pyrrole-2-carbonyl)piperidine-4-carboxylic acid

생성물 1

HCID 66571158HCID 66571158, 화합물수율 69.8%

시약·촉매·용매 3

HCID 3283Diethyl Ether용매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

The following was dissolved in anhydrous DMF (3 mL): 1-(1-(4-chlorobenzyl)-1H-pyrrole-2-carbonyl)piperidine-4-carboxylic acid (115 mg, 0.332 mmol), Hunig's Base (0.174 ml, 0.995 mmol), EDC (76 mg, 0.398 mmol), HOBt (60.9 mg, 0.398 mmol), and benzylamine (0.040 ml, 0.365 mmol). This was stirred at room temperature for 1 day with 3 Å molecular sieves. At this time, a 1:1 solution of EtOAc:Et2O (20 mL) was added and the organic layer was washed with 10% aq. Na2CO3 (2×10 mL) and brine (1×10 mL). The organic solution was then dried (anhydrous MgSO4) and concentrated in vacuo. Trituration in Et2O provided 101 mg of the title compound as a fine, ruddy brown solid.

후처리

  1. washthe organic layer was washed with 10% aq. Na2CO3 (2×10 mL) and brine (1×10 mL)
  2. dry with materialThe organic solution was then dried (anhydrous MgSO4)
  3. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-d09c387e53d24c20a5fb537a9453b272
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846684B2

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