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Diethyl Ether → HCID 13020484, 화합물

HRID 2198520
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HRID 2198520 반응식
Cl.[CH:2]1([CH2:15][C:16]([O:18]CC)=O)[C:7]2[NH:8][C:9]3[C:14]([C:6]=2[CH2:5][CH2:4][NH:3]1)=[CH:13][CH:12]=[CH:11][CH:10]=3.[O-:21][C:22]#[N:23].[Na+].[CH3:25]COCC>O>[CH3:25][N:23]1[C:16](=[O:18])[CH2:15][CH:2]2[C:7]3[NH:8][C:9]4[C:14]([C:6]=3[CH2:5][CH2:4][N:3]2[C:22]1=[O:21])=[CH:13][CH:12]=[CH:11][CH:10]=4
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5

반응물 3

HCID 3283Diethyl Ether2회HCID 517096Sodium CyanateHCID 20519381Ethyl (2,3,4,9-tetrahydro-1H-beta-carbolin-1-yl)acetate--hydrogen chloride (1/1)

생성물 1

HCID 13020484HCID 13020484, 화합물

시약·촉매·용매 1

HCID 962Water용매3회

실험 절차

26 g (0.088 mol) of ethyl 2,3,4,9-tetrahydro-1H-pyrido[3,4-b]indole-1-acetate hydrochloride are dissolved in 1 liter of hot water. The pH should be 4-5. When the temperature of the reaction medium is 50° C., a solution of 8.7 g (0.13 mol) of sodium cyanate in 150 cm3 of water is added. The reaction medium is kept at 50° C., whilst stirring. It is stirred for 4 hours at 50° C. and left to stand overnight at ambient temperature; the supernatant water is drawn off. 200 cm3 of ether are added, the mixture is stirred, the ether solution is then drawn off and the same operation is repeated. The expected product is very soluble in ether. The ether extracts are combined and washed with acidified water, in order to remove traces of the starting material, and then with water. They are dried over Na2SO4 and the solvent is evaporated off. This yields an oil which changes into a foam on more thorough drying. The product is used as such in the following step.

후처리

  1. customis 50° C.
  2. customis kept at 50° C.
  3. stirringIt is stirred for 4 hours at 50° C.
  4. waitleft
  5. stirringthe mixture is stirred

출처 및 근거

ORD 기록
ord-38cb2051bbe54cafbf743a4aff7f164f
출처 데이터셋
uspto-grants-1982_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04358451

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