Triethylamine → HCID 178491487、化合物

HRID 133794

反応式

HRID 133794 の反応式
[OH:1][CH:2]([C:7]1[CH:12]=[CH:11][C:10]([O:13][CH3:14])=[CH:9][CH:8]=1)[CH2:3][C:4]([OH:6])=O.[C:15]([NH:18][C:19]1[C:36]([Cl:37])=[CH:35][C:22]([CH2:23][NH:24]/[C:25](/[NH2:34])=[N:26]\[C:27](=[O:33])[O:28][C:29]([CH3:32])([CH3:31])[CH3:30])=[CH:21][C:20]=1[Cl:38])(=[O:17])[CH3:16].C1CN([P+](ON2N=NC3C=CC=CC2=3)(N2CCCC2)N2CCCC2)CC1.F[P-](F)(F)(F)(F)F.C(N(CC)CC)C>ClCCl>[C:15]([NH:18][C:19]1[C:20]([Cl:38])=[CH:21][C:22]([CH2:23][NH:24]/[C:25](=[N:26]\[C:27](=[O:33])[O:28][C:29]([CH3:31])([CH3:32])[CH3:30])/[NH:34][C:4](=[O:6])[CH2:3][CH:2]([OH:1])[C:7]2[CH:12]=[CH:11][C:10]([O:13][CH3:14])=[CH:9][CH:8]=2)=[CH:35][C:36]=1[Cl:37])(=[O:17])[CH3:16]

参加物

6

反応物 4

HCID 8471TriethylamineHCID 2724699PyBOPHCID 149273073-Hydroxy-3-(4-methoxyphenyl)propanoic acidHCID 178474312HCID 178474312、化合物

生成物 1

HCID 178491487HCID 178491487、化合物収率 77.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 3-hydroxy-3-(4-methoxyphenyl)propanoic acid (13.7 mg, 0.07 mmol), (Z)-tert-butyl (4-acetamido-3,5-dichlorobenzylamino)(amino)-methylenecarbamate (26.3 mg), PyBop (36.4 mg), and triethylamine (0.01 mL) in dichloromethane (0.35 mL) was stirred at room temperature for 12 h. The crude reaction mixture was purified directly by preparative TLC eluting with 30% ethyl acetate/70% hexanes to give the title compound as a clear sticky oil (30 mg, 77% yield). 1H NMR (400 MHz, CDCl3) δ 1.48 (m, 9 H) 2.21 (s, 3 H) 2.70 (m, 2 H) 3.78 (m, 3 H) 4.55 (m, 2 H) 4.95 (m, 1 H) 6.80-7.00 (m, 3 H) 7.24-7.38 (m, 4 H), 9.10 (m, 1 H), 12.30 (m, 1 H). HPLC retention time: 2.493 min (method A). MS (ESI) (M+H)+ 553.08.

後処理

  1. customThe crude reaction mixture
  2. customwas purified directly by preparative TLC
  3. washeluting with 30% ethyl acetate/70% hexanes

出典と根拠

ORDレコード
ord-e2bed52f21754bca906fd61d26a1a75a
出典データセット
uspto-grants-2008_06
特許番号
US07390925B2

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