Diethyl Ether → HCID 22220851, 화합물

HRID 1794036노트

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HRID 1794036 반응식
[S:1]1[CH:5]=[CH:4][N:3]=[C:2]1[CH:6]([OH:8])[CH3:7].[Cl:9][CH2:10][C:11]([N:13]1[CH2:17][CH2:16][CH2:15][CH2:14]1)=[O:12].C(#N)C.CCOCC>CO>[Cl-:9].[OH:8][CH:6]([C:2]1[S:1][CH:5]=[CH:4][N+:3]=1[CH2:10][C:11](=[O:12])[N:13]1[CH2:17][CH2:16][CH2:15][CH2:14]1)[CH3:7]

참가 물질

6

반응물 4

HCID 3283Diethyl EtherHCID 6342Acetonitrile2회HCID 884401-(Chloroacetyl)pyrrolidineHCID 99892951-(1,3-Thiazol-2-yl)ethan-1-ol

생성물 1

HCID 22220851HCID 22220851, 화합물수율 66.9%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

1-(2-Thiazolyl)ethanol (1.14 g, 8.8 mmole), N-chloroacetylpyrrolidine (1.30 g, 8.8 mmole), and acetonitrile (1.25 mL) were combined and heated at reflux in an oil bath at 105–110 C for 6 hr. Acetonitrile (8 mL) was added and heating was continued 10 min. The cooled, clear solution was treated with ether (10 mL), causing an oil to separate, which crystalized on standing at room temp. overnight. Filtration and washing with 30% ether/acetonitrile gave 1.86 g crude product which was dissolved in methanol, decolorized, and evaporated to dryness. The residue was recrystalized from acetonitrile/ether and from methanol/acetonitrile/ether to yield 1.63 g of the title compound, mp 189–190 C (dec.).

후처리

  1. temperatureheated
  2. temperatureat reflux in an oil bath at 105–110 C for 6 hr
  3. temperatureheating
  4. customto separate
  5. customwhich crystalized
  6. waiton standing at room temp. overnight
  7. filtrationFiltration
  8. washwashing with 30% ether/acetonitrile
  9. customgave 1.86 g crude product which
  10. customevaporated to dryness
  11. customThe residue was recrystalized from acetonitrile/ether and from methanol/acetonitrile/ether

출처 및 근거

ORD 기록
ord-39ba1c4ef4d3464e979d8a9240055043
출처 데이터셋
uspto-grants-2006_04
특허 번호
US07022721B1

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