1,2-Dichloroethane → HCID 67264809, 화합물

HRID 1685117노트

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HRID 1685117 반응식
[NH2:1][CH2:2][C@H:3]1[N:8]([CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH2:7][CH2:6][N:5]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:4]1.[C:23](O)(=[O:30])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.C(Cl)CCl.CCN(C(C)C)C(C)C>ClCCl>[C:23]([NH:1][CH2:2][C@H:3]1[N:8]([CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH2:7][CH2:6][N:5]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:4]1)(=[O:30])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

참가 물질

6

반응물 4

HCID 111,2-DichloroethaneHCID 243Benzoic AcidHCID 81531DiisopropylethylamineHCID 57415720tert-Butyl (3R)-3-(aminomethyl)-4-benzylpiperazine-1-carboxylate

생성물 1

HCID 67264809HCID 67264809, 화합물수율 79%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

Into a 50 mL round bottom flask was added 15S (820 mg, 2.68 mmol) and dichloromethane (15 mL). Benzoic acid (15T) (426 mg, 1.3 eq) and EDC (669 mg, 1.3 eq) was added and the flask was cooled to 0° C. DIEA (1.04 g, 3 equiv.) was slowly added and the reaction was stirred at room temperature overnight. The solvent was removed under vacuum and the residue was purified by column chromatography with 5% methanol in dichloromethane to give 15U as a solid (865 mg, 79%).

후처리

  1. customThe solvent was removed under vacuum
  2. customthe residue was purified by column chromatography with 5% methanol in dichloromethane

출처 및 근거

ORD 기록
ord-e62b1632ec91467cbfcaff3b8013fed3
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08148367B2

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