Triethylamine → HCID 19069744, 화합물

HRID 1957321노트

반응식

HRID 1957321 반응식
[CH2:1]([NH:3][CH2:4][C:5]([OH:7])=O)[CH3:2].[F:8][C:9]1[CH:14]=[CH:13][C:12]([CH:15]([N:17]=[C:18]=[S:19])[CH3:16])=[CH:11][CH:10]=1.C(N(CC)CC)C>C(Cl)(Cl)Cl>[CH2:1]([N:3]1[CH2:4][C:5](=[O:7])[N:17]([CH:15]([C:12]2[CH:13]=[CH:14][C:9]([F:8])=[CH:10][CH:11]=2)[CH3:16])[C:18]1=[S:19])[CH3:2]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 316542N-EthylglycineHCID 5195361-Fluoro-4-(1-isothiocyanatoethyl)benzene

생성물 1

HCID 19069744HCID 19069744, 화합물수율 33.1%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

A mixture of the crude N-ethyl glycine (18.4 g), 1-(4-fluorophenyl)-ethyl-isothiocyanate (18.1 g), triethyl amine (20.2 g) and chloroform (300 mL) was heated at reflux for 18 hours. The solvent was evaporated. The residue was dissolved in ethyl acetate (400 mL) and water (300 mL). The organic phase was washed with 1N HCl (2×300 mL), then evaporated to dryness. Crystallization from ethyl acetate afforded the title compound (8.8 g) as a light yellow solid, m.p. 93°-95° C. Anal. Calcd. for. C13H15F N2O S: C, 58.63; H, 5.68; N, 10.52. Found: C, 58.69; H, 5.64; N, 10.58. Mass spectrum (EI, M.+) m/z 266.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 18 hours
  3. customThe solvent was evaporated
  4. dissolutionThe residue was dissolved in ethyl acetate (400 mL)
  5. washThe organic phase was washed with 1N HCl (2×300 mL)
  6. customevaporated to dryness
  7. customCrystallization from ethyl acetate

출처 및 근거

ORD 기록
ord-5cee7a7d2cbc49778c00551f354cc2b6
출처 데이터셋
uspto-grants-1998_07
특허 번호
US05783707

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