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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Ethylenediamine → HCID 13715489, 화합물

HRID 1165180
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HRID 1165180 반응식
C[Al](C)C.[CH2:5]([NH2:8])[CH2:6][NH2:7].C(O[C:12]([CH:14]1[CH2:22][C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[N:15]1[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)=O)C>C1(C)C=CC=CC=1>[NH:7]1[CH2:6][CH2:5][N:8]=[C:12]1[CH:14]1[CH2:22][C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[N:15]1[C:23]1[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 3301EthylenediamineHCID 13869736HCID 13869736, 화합물HCID 16682925Trimethylaluminum

생성물 1

HCID 13715489HCID 13715489, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

To a stirring solution of 2 molar trimethylaluminum in toluene (13.1 ml) at 10° C. under argon is added ethylenediamine (1.75 ml) dropwise under cooling to maintain a temperature of +10° C. It is allowed to ware to room temperature and then ethyl-2,3-dihydro-1-phenylindole-2-carboxylate (3.5 g) in toluene (15 ml) is added under argon. The whole is heated gradually to reflux and maintained at this temperature under argon for 18 hours. This cooled mixture is quenched in water (40 ml) and treated with methanol (40 ml) and methylene chloride (40 ml). The aqueous layer is separated and extracted further with methylene chloride (3×100 ml). The combined organic extracts are dried over sodium sulfate and concentrated to dryness at reduced pressure. The residue is dissolved in boiling ethyl acetate (150 ml), filtered through sodiumsulfate and concentrated to reduced pressure to a small volume from which yellow solid precipitates. The pure dl-2,3-dihydro-2-(4,5-dihydroimidazol-2-yl)-1-phenylindole, mp. 141° -144°, is thus obtained.

후처리

  1. temperatureunder cooling
  2. temperatureto maintain a temperature of +10° C
  3. customto ware to room temperature
  4. temperatureThe whole is heated gradually
  5. temperatureto reflux
  6. temperaturemaintained at this temperature under argon for 18 hours
  7. customThis cooled mixture is quenched in water (40 ml)
  8. additiontreated with methanol (40 ml) and methylene chloride (40 ml)
  9. customThe aqueous layer is separated
  10. extractionextracted further with methylene chloride (3×100 ml)
  11. dry with materialThe combined organic extracts are dried over sodium sulfate
  12. concentrationconcentrated to dryness at reduced pressure
  13. dissolutionThe residue is dissolved
  14. filtrationfiltered through sodiumsulfate
  15. concentrationconcentrated to reduced pressure to a small volume from which yellow solid
  16. customprecipitates

출처 및 근거

ORD 기록
ord-74c2367568ab4b3bb0d5d4f5a0cc9f62
출처 데이터셋
uspto-grants-1990_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04908376

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