Oxalyl chloride → HCID 57796889, 화합물

HRID 2099960

반응식

HRID 2099960 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

HCID 57796889HCID 57796889, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide촉매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-69fd503af22c4d219c7e558793126094
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07569725B2

연결된 노트

불러오는 중…