Oxalyl chloride → Ethyl 2-(4-(3,4-dimethoxybenzyloxy)-3-chlorobenzamido)-5-phenoxybenzoate

HRID 2099960

反応式

HRID 2099960 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:18]=[CH:19][C:20]=1[O:21][CH3:22])[CH2:6][O:7][C:8]1[CH:16]=[CH:15][C:11]([C:12]([OH:14])=O)=[CH:10][C:9]=1[Cl:17].C(Cl)(=O)C(Cl)=O.[NH2:29][C:30]1[CH:40]=[CH:39][C:38]([O:41][C:42]2[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=2)=[CH:37][C:31]=1[C:32]([O:34][CH2:35][CH3:36])=[O:33].C(N(C(C)C)CC)(C)C>C(Cl)Cl.CN(C=O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:18]=[CH:19][C:20]=1[O:21][CH3:22])[CH2:6][O:7][C:8]1[CH:16]=[CH:15][C:11]([C:12]([NH:29][C:30]2[CH:40]=[CH:39][C:38]([O:41][C:42]3[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=3)=[CH:37][C:31]=2[C:32]([O:34][CH2:35][CH3:36])=[O:33])=[O:14])=[CH:10][C:9]=1[Cl:17]

参加物

7

反応物 4

HCID 65578Oxalyl chlorideHCID 81531DiisopropylethylamineHCID 57796887HCID 57796887、化合物HCID 577968974-(3,4-Dimethoxybenzyloxy)-3-chlorobenzoic acid

生成物 1

HCID 57796889Ethyl 2-(4-(3,4-dimethoxybenzyloxy)-3-chlorobenzamido)-5-phenoxybenzoate

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide触媒HCID 6344Dichloromethane溶媒

実験手順

A solution of 1B (200 mg, 0.62 mmol) in CH2Cl2 (10 mL) was cooled to 0° C. and treated with several drops of DMF. Oxalyl chloride was added dropwise over 10 minutes. The resulting solution was stirred for 10 minutes, and then concentrated to dryness. The resulting solid was dissolved in CH2Cl2 (10 mL) and treated with ethyl 2-amino-5-phenoxybenzoate (144 mg, 0.56 mmol) and diisopropylethylamine (130 μL, 0.74 mmol). The reaction was stirred at room temperature for 3 hours and then concentrated to afford 1C as a white solid.

後処理

  1. concentrationconcentrated to dryness
  2. dissolutionThe resulting solid was dissolved in CH2Cl2 (10 mL)
  3. stirringThe reaction was stirred at room temperature for 3 hours
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-69fd503af22c4d219c7e558793126094
出典データセット
uspto-grants-2009_08
特許番号
US07569725B2

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