1,2-Dichloroethane → HCID 86752943、化合物

HRID 1957578ノート

反応式

HRID 1957578 の反応式
[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]

参加物

7

反応物 5

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 10752421HCID 10752421、化合物HCID 19068157HCID 19068157、化合物

生成物 1

HCID 86752943HCID 86752943、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-b3f4d268f50e4a6ebde81f2d924c1219
出典データセット
uspto-grants-1998_07
特許番号
US05786373

反応ノート

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