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Potassium Carbonate → HCID 21072863, 화합물

HRID 1867317
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HRID 1867317 반응식
[C:1]([C:4]1[C:5]([OH:25])=[C:6]([NH:18][C:19](=[O:24])[C:20](Br)([CH3:22])[CH3:21])[CH:7]=[C:8]([O:10][CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:9]=1)(=[O:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[C:1]([C:4]1[C:5]2[O:25][C:20]([CH3:22])([CH3:21])[C:19](=[O:24])[NH:18][C:6]=2[CH:7]=[C:8]([O:10][CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:9]=1)(=[O:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 21072865N-(3-acetyl-5-benzyloxy-2-hydroxyphenyl)-2-bromo-2-methylpropionamide

생성물 1

HCID 21072863HCID 21072863, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

6.60 g (16.2 mmol) of N-(3-acetyl-5-benzyloxy-2-hydroxyphenyl)-2-bromo-2-methylpropionamide and 2.76 g (20 mmol) of potassium carbonate are stirred for 1 hour in 70 mL acetonitrile at reflux temperature. The solid is suction filtered, the filtrate is evaporated down, and the residue is combined with 30 mL of ethyl acetate. After fresh filtration and distilling off the solvent, the crude product is crystallized from a little methanol. Yield: 1.00 g (19%); mass spectroscopy [M+H]+=326; melting range=148° C.-150° C.

후처리

  1. temperatureat reflux temperature
  2. filtrationfiltered
  3. customthe filtrate is evaporated down
  4. filtrationAfter fresh filtration
  5. distillationdistilling off the solvent
  6. customthe crude product is crystallized from a little methanol

출처 및 근거

ORD 기록
ord-6733d131e8784ce4a5c4ed61bf3e1eb0
출처 데이터셋
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07632834B2

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