Dipropylamine → 2-[2-(2,2-dimethylpropanoyl)-5-methoxy-1-benzofuran-3-yl]-N,N-dipropylacetamide

HRID 2103756

반응식

HRID 2103756 반응식
[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](O)=[O:12])=[O:4].C1C=CC2N(O)N=NC=2C=1.[CH2:32]([NH:35][CH2:36][CH2:37][CH3:38])[CH2:33][CH3:34].CCN(C(C)C)C(C)C>CN(C=O)C.C(Cl)CCl>[CH3:21][C:2]([CH3:20])([CH3:1])[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:35]([CH2:36][CH2:37][CH3:38])[CH2:32][CH2:33][CH3:34])=[O:12])=[O:4]

참가 물질

7

반응물 4

HCID 8902DipropylamineHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 57804476[2-(2,2-Dimethylpropanoyl)-5-methoxy-1-benzofuran-3-yl]acetic acid

생성물 1

HCID 112341532-[2-(2,2-dimethylpropanoyl)-5-methoxy-1-benzofuran-3-yl]-N,N-dipropylacetamide

시약·촉매·용매 2

HCID 111,2-Dichloroethane용매HCID 6228Dimethylformamide용매

반응 조건

온도
40 °C

실험 절차

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 12.1 μL dipropylamine 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 60-100% MeCN gradient. The fractions containing pure product were pooled and lyophilized to give the title compound. LC-MS: 4.16 min. (m/Z=290.1, 374.2, 396.1).

후처리

  1. dissolutionDissolve
  2. customIt was purified directly on RP-HPLC using 60-100% MeCN gradient
  3. additionThe fractions containing pure product

출처 및 근거

ORD 기록
ord-d5b7f657d063409b94fdb5e6ebe1de47
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07576122B2

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