1,2-Dichloroethane → HCID 67264809、化合物

HRID 1685117ノート

反応式

HRID 1685117 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 67264809HCID 67264809、化合物収率 79%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

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%).

後処理

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

出典と根拠

ORDレコード
ord-e62b1632ec91467cbfcaff3b8013fed3
出典データセット
uspto-grants-2012_04
特許番号
US08148367B2

反応ノート

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