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Diethylaminopropyl chloride, hydrochloride → HCID 20312101, 화합물

HRID 2420533
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HRID 2420533 반응식
[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]([CH:10]2[NH:14][C:13](=[O:15])[NH:12][C:11]2=[O:16])=[CH:2]1.[Na].Cl.[CH2:19]([N:21]([CH2:26][CH3:27])[CH2:22][CH2:23][CH2:24]Cl)[CH3:20]>CN(C=O)C.C(O)C>[CH2:19]([N:21]([CH2:26][CH3:27])[CH2:22][CH2:23][CH2:24][N:12]1[C:11](=[O:16])[CH:10]([C:3]2[C:4]3[C:9](=[CH:8][CH:7]=[CH:6][CH:5]=3)[NH:1][CH:2]=2)[NH:14][C:13]1=[O:15])[CH3:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 145749Diethylaminopropyl chloride, hydrochlorideHCID 5360545SodiumHCID 20186934HCID 20186934, 화합물

생성물 1

HCID 20312101HCID 20312101, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 6228Dimethylformamide용매

실험 절차

A solution of 5-(indol-3-yl)hydantoin (5.2 g, 0.024 mole) in 100 ml of DMF was added to a solution of sodium (1.1 g) in 100 ml of anhydrous C2H5OH. The solution was warmed warmed 3-diethylaminopropyl chloride hydrochloride (4.5 g, 0.024 mole) was added and the mixture was heated to reflux with stirring for 18 hours, filtered and diluted with H2O. The crude free base (2.5 g) and oxalic acid (1.5 g) was dissolved in methanol and diluted with ethyl acetate. The solid was collected and dried, yield 1.0 g, mp 231°-2°.

후처리

  1. temperatureThe solution was warmed
  2. additionwas added
  3. temperaturethe mixture was heated
  4. temperatureto reflux
  5. filtrationfiltered
  6. additiondiluted with H2O
  7. dissolutionThe crude free base (2.5 g) and oxalic acid (1.5 g) was dissolved in methanol
  8. additiondiluted with ethyl acetate
  9. customThe solid was collected
  10. customdried

출처 및 근거

ORD 기록
ord-ecfb866d4c014cafab2f947fd987af3b
출처 데이터셋
uspto-grants-1978_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04110536

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