Diisobutylamine → 2-[2-(2,2-Dimethylpropanoyl)-5-methoxy-1-benzofuran-3-yl]-N,N-diisobutylacetamide

HRID 2103753

反応式

HRID 2103753 の反応式
[CH3:1][C:2]([CH3:21])([CH3:20])[C:3]([C:5]1[O:6][C:7]2[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][C:8]=2[C:9]=1[CH2:10][C:11]([OH:13])=O)=[O:4].C1C=CC2N(O)N=NC=2C=1.[CH2:32]([NH:36][CH2:37][CH:38]([CH3:40])[CH3:39])[CH:33]([CH3:35])[CH3:34].CCN(C(C)C)C(C)C>CN(C=O)C.C(Cl)CCl>[CH3:1][C:2]([CH3:20])([CH3:21])[C:3]([C:5]1[O:6][C:7]2[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][C:8]=2[C:9]=1[CH2:10][C:11]([N:36]([CH2:37][CH:38]([CH3:40])[CH3:39])[CH2:32][CH:33]([CH3:35])[CH3:34])=[O:13])=[O:4]

参加物

7

反応物 4

HCID 8085DiisobutylamineHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 57804476[2-(2,2-Dimethylpropanoyl)-5-methoxy-1-benzofuran-3-yl]acetic acid

生成物 1

HCID 113501542-[2-(2,2-Dimethylpropanoyl)-5-methoxy-1-benzofuran-3-yl]-N,N-diisobutylacetamide

試薬・触媒・溶媒 2

HCID 111,2-Dichloroethane溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
40 °C

実験手順

Dissolve a mixture of 17 mg [2-(2,2-dimethylpropanoyl)-5-methoxy-1-benzofuran-3-yl]acetic acid from the Step B Example 1 and 18.5 mg HOBt in 1 mL dry DMF. Add 15.4 μL di-i-butylamine followed by 23.0 mg EDC and 35 μL DIEA. This solution was heated at 40° C. for 2 hours. It was purified directly on RP-HPLC using 65-100% MeCN gradient. The fractions containing pure product were pooled and lyophilized to give the title compound. LC-MS: 4.42 min. (m/Z=318.2, 402.2, 424.2).

後処理

  1. dissolutionDissolve
  2. customIt was purified directly on RP-HPLC using 65-100% MeCN gradient
  3. additionThe fractions containing pure product

出典と根拠

ORDレコード
ord-85e94175ff08464a9636651522046be1
出典データセット
uspto-grants-2009_08
特許番号
US07576122B2

関連ノート

読み込み中…