1,2-Dichloroethane → HCID 86752943, 화합물

HRID 1957578노트

반응식

HRID 1957578 반응식
[C:1]([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][CH2:15][CH2:16][O:17][C:18]2[CH:22]=[C:21]([C:23]([OH:25])=O)[O:20][N:19]=2)[CH2:10][CH2:9]1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].[NH2:26][CH2:27][C@H:28]([NH:33][S:34]([CH2:37][CH2:38][CH2:39][CH3:40])(=[O:36])=[O:35])[C:29]([O:31][CH3:32])=[O:30].C1C=CC2N(O)N=NC=2C=1.N(CC)(C(C)C)C(C)C.C(Cl)CCl>CN(C=O)C>[CH3:32][O:31][C:29](=[O:30])[C@@H:28]([NH:33][S:34]([CH2:37][CH2:38][CH2:39][CH3:40])(=[O:36])=[O:35])[CH2:27][NH:26][C:23]([C:21]1[O:20][N:19]=[C:18]([O:17][CH2:16][CH2:15][CH2:14][CH:11]2[CH2:10][CH2:9][N:8]([C:1]([O:3][C:4]([CH3:7])([CH3:5])[CH3:6])=[O:2])[CH2:13][CH2:12]2)[CH:22]=1)=[O:25]

참가 물질

7

반응물 5

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 10752421HCID 10752421, 화합물HCID 19068157HCID 19068157, 화합물

생성물 1

HCID 86752943HCID 86752943, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A stirred solution of 3-7 (142 mg, 0.4 mmol), 2-9 (110 mg, 0.4 mmol), HOBT (61 mg, 0.4 mmol), N(i-Pr)2Et (216 μL, 1.2 mmol) and DMF (7 mL) at -15° C. was treated with EDC (77 mg, 0.4 mmol) followed by removal of the cooling bath. After 20 h. the reaction mixture concentrated followed by dilution with EtOAc. The EtOAc solution was washed with 1M NaHSO4, and brine, dried (MgSO4), and concentrated. Flash chromatography (silica, 10% to 20% acetone/CH2Cl2) to give 3-8 as a viscous gum. Rf 0.64 (silica, 20% acetone/CH2Cl2).

후처리

  1. customfollowed by removal of the cooling bath
  2. concentrationAfter 20 h. the reaction mixture concentrated
  3. washThe EtOAc solution was washed with 1M NaHSO4, and brine
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-b3f4d268f50e4a6ebde81f2d924c1219
출처 데이터셋
uspto-grants-1998_07
특허 번호
US05786373

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