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Water → HCID 59520429, 화합물

HRID 1162517
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HRID 1162517 반응식
[Cl:1][C:2]1[CH:11]=[C:10]([Cl:12])[CH:9]=[CH:8][C:3]=1[O:4][CH2:5][CH2:6][NH2:7].[CH3:13][O:14][C:15](=[O:33])[CH2:16][C:17]1[CH:22]=[CH:21][C:20]([C:23]2[C:27]([C:28](Cl)=[O:29])=[C:26]([CH3:31])[O:25][N:24]=2)=[C:19]([Cl:32])[CH:18]=1.C(N(CC)CC)C.O>C1(C)C=CC=CC=1.CC#N>[CH3:13][O:14][C:15](=[O:33])[CH2:16][C:17]1[CH:22]=[CH:21][C:20]([C:23]2[C:27]([C:28](=[O:29])[NH:7][CH2:6][CH2:5][O:4][C:3]3[CH:8]=[CH:9][C:10]([Cl:12])=[CH:11][C:2]=3[Cl:1])=[C:26]([CH3:31])[O:25][N:24]=2)=[C:19]([Cl:32])[CH:18]=1
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참가 물질

7

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 1508972-(2,4-Dichlorophenoxy)ethylamineHCID 59520424HCID 59520424, 화합물

생성물 1

HCID 59520429HCID 59520429, 화합물

시약·촉매·용매 2

HCID 1140Toluene용매
HCID 6342
Acetonitrile
용매

실험 절차

A solution of 2-(2,4-Dichloro-phenoxy)-ethylamine 29 (17 mg, 0.08 mmol) in toluene (2 mL) is cooled to 0° C. A solution of intermediate 26 (0.08 mmol) and triethylamine (23 μL, 0.16 mmol) in MeCN (1 mL) is added and the solution is warmed to room temperature. After stirring at room temperature for 1 h the mixture is poured into H2O and extracted three times with EtOAc. The organic layers are combined, dried (MgSO4), filtered, and concentrated to afford crude (3-Chloro-4-{4-[2-(2,4-dichloro-phenoxy)-ethylcarbamoyl]-5-methyl-isoxazol-3-yl}-phenyl)-acetic acid methyl ester 30.

후처리

  1. extractionextracted three times with EtOAc
  2. dry with materialdried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-f4cc71de5f154dccbefd3921e4a5197b
출처 데이터셋
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07820705B2

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