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Sodium Hydroxide → HCID 20566612, 화합물

HRID 1577949
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HRID 1577949 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([NH:17]C(=O)N(C)C)[CH:5]=[CH:6][C:7]=1[O:8][CH2:9][CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[OH-].[Na+]>C(O)CCC>[ClH:1].[Cl:1][C:2]1[CH:3]=[C:4]([CH:5]=[CH:6][C:7]=1[O:8][CH2:9][CH2:10][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1)[NH2:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 129420803-[3-Chloro-4-(phenethyloxy)phenyl]-1,1-dimethylurea

생성물 1

HCID 20566612HCID 20566612, 화합물수율 140.7%

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

A mixture of 3-[3-chloro-4-(phenethyloxy) phenyl]-1,1-dimethylurea (16.68 g; 0.0523 mol), n-butanol (300 ml) and 50% aqueous sodium hydroxide (50 ml) is refluxed for 1.5 hours, and then poured onto 500 ml crushed ice. The resultant mixture is extracted with ether (2×200 ml). The ether solution is washed with brine, dried over potassium carbonate and cooled in an ice bath. Dry hydrochloric acid gas is bubbled through the solution. The precipitated amine hydrochloride is collected to afford 10.46 g (0.0368 mol) of product, a white solid, m.p. 198°-204° C.

후처리

  1. temperatureis refluxed for 1.5 hours
  2. additionpoured onto 500 ml
  3. customcrushed ice
  4. extractionThe resultant mixture is extracted with ether (2×200 ml)
  5. washThe ether solution is washed with brine
  6. dry with materialdried over potassium carbonate
  7. temperaturecooled in an ice bath
  8. customDry hydrochloric acid gas is bubbled through the solution
  9. customThe precipitated amine hydrochloride is collected

출처 및 근거

ORD 기록
ord-540241e1861a430aaacbcc72ce6c1643
출처 데이터셋
uspto-grants-1981_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04289903

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