Hydrochloric Acid → Hydrate;dihydrochloride

HRID 918365노트

반응식

HRID 918365 반응식
[ClH:1].[C:2]([CH:4]1[C:16]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[C:10]2[C:5]1=[CH:6][CH:7]=[CH:8][CH:9]=2)#[N:3].[CH2:17]([OH:19])[CH3:18]>CCOCC>[CH2:17]([O:19][C:2]([CH:4]1[C:16]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[C:10]2[C:5]1=[CH:6][CH:7]=[CH:8][CH:9]=2)=[NH:3])[CH3:18].[OH2:19].[ClH:1].[ClH:1]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 737219H-Fluorene-9-carbonitrile

생성물 2

HCID 21226127Hydrate;dihydrochlorideHCID 542542839H-Fluorene-9-carboximidic acid ethyl ester

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

Dry hydrogen chloride was passed for 3 hours into a solution of 9-cyanofluorene (15 67.85; g.; see, for example, J. Amer. Chem. Soc., 1949, 71, 1500) in ether (1 l.) ans absolute ethanol (45 ml.) at 0°C. The mixture was left at 0°C overnight, the solid filtered, washed with ether and dried under vacuum at room temperature to give the title compound as its hydrochloride hemihydrate (17.61 g., m.p. 262°-263°C dec.). Found: C, 68.5; H, 6.05; N, 4.95%. C16H13NO.HCl.1/2H2O requires C, 687.85; H, 6.05; N, 4.95%.

후처리

  1. customat 0°C
  2. filtrationthe solid filtered
  3. washwashed with ether
  4. customdried under vacuum at room temperature

출처 및 근거

ORD 기록
ord-0a5d8286d7bc4bd49403ed3a138078c5
출처 데이터셋
uspto-grants-1976_07
특허 번호
US03971782

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