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Triethylamine → HCID 21867225, 화합물

HRID 857159
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HRID 857159 반응식
[CH3:1][O:2][C:3](=[O:28])[CH2:4][C:5]1[CH:10]=[C:9]([Cl:11])[C:8]([O:12][C:13]2[CH:18]=[CH:17][C:16]([NH:19][CH2:20][C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)=[CH:15][CH:14]=2)=[C:7]([Cl:27])[CH:6]=1.C(N(CC)CC)C.[C:36](Cl)(=[O:40])[CH:37]([CH3:39])[CH3:38]>ClCCl>[CH3:1][O:2][C:3](=[O:28])[CH2:4][C:5]1[CH:10]=[C:9]([Cl:11])[C:8]([O:12][C:13]2[CH:14]=[CH:15][C:16]([N:19]([C:36](=[O:40])[CH:37]([CH3:39])[CH3:38])[CH2:20][C:21]3[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=3)=[CH:17][CH:18]=2)=[C:7]([Cl:27])[CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 62325Isobutyryl chlorideHCID 21867255Methyl[3,5-dichloro-4-(4-benzylaminophenoxy)phenyl]acetate

생성물 1

HCID 21867225HCID 21867225, 화합물수율 95.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a stirred mixture of methyl[3,5-dichloro-4-(4-benzylaminophenoxy)phenyl]acetate (0.36 g), triethylamine (0.10 g) and dichloromethane (40 mL) was added isobutyryl chloride (0.15 g). After 16 hours at room temperature, the reaction mixture was concentrated, and the residue partioned between ethyl acetate and water. The organic phase was washed with hydrochloric acid (1 N), a saturated aqueous solution of sodium hydrogencarbonate and brine. After concentration, the residue was purified on column (silica gel, petrolium ether/ethyl acetate, 4:1) to give, to give 0.40 g of methyl[3,5-dichloro-4-(4-(2-methylpropanoyl-benzylamino)phenoxy)phenyl]acetate.

후처리

  1. concentrationthe reaction mixture was concentrated
  2. washThe organic phase was washed with hydrochloric acid (1 N)
  3. concentrationAfter concentration
  4. customthe residue was purified on column (silica gel, petrolium ether/ethyl acetate, 4:1)
  5. customto give

출처 및 근거

ORD 기록
ord-9ab1c2dfbffe470dbb877b766a4f2d38
출처 데이터셋
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07144909B2

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