1-Butanol → HCID 178450655, 화합물

HRID 346292

반응식

HRID 346292 반응식
[C:1]([C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9]([CH3:14])([CH3:13])[CH2:8][CH2:7][C:6]2([CH3:16])[CH3:15])#[CH:2].[CH:17]([C:19]1[CH:28]=[CH:27][C:22]([C:23]([O:25][CH3:26])=[O:24])=[CH:21][CH:20]=1)=O.[NH2:29][C:30]([NH2:32])=[O:31].S(=O)(=O)(O)O.[CH2:38](O)[CH2:39][CH2:40]C>CCOCC.O>[C:23]([C:22]1[CH:27]=[CH:28][C:19]([C:17]2[CH:2]=[C:1]([C:3]3[CH:12]=[CH:11][C:10]4[C:9]([CH3:14])([CH3:13])[CH2:8][CH2:7][C:6]([CH3:16])([CH3:15])[C:5]=4[CH:4]=3)[N:32]=[C:30]([OH:31])[N:29]=2)=[CH:20][CH:21]=1)([O:25][CH2:26][CH2:38][CH2:39][CH3:40])=[O:24]

참가 물질

8

반응물 5

HCID 2631-ButanolHCID 1118Sulfuric AcidHCID 1176UreaHCID 15294Methyl 4-FormylbenzoateHCID 147265491,1,4,4-Tetramethyl-6-ethynyl-1,2,3,4-tetrahydronaphthalene

생성물 1

HCID 178450655HCID 178450655, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 3283Diethyl Ether용매

실험 절차

21 g (0.1 mole) of 6-ethynyl-1,2,3,4-tetrahydro-1,1,4,4-tetramethylnaphthalene, 16 g (0.1 mole) of methyl 4-formylbenzoate, 9 g (0.15 mole) of urea and 15 ml of concentrated sulfuric acid in 50 ml of n-butanol were refluxed for 4 hours. After cooling, the mixture was poured onto 500 ml of water, 100 ml of ether were added and stirring was carried out for 5 minutes. A solid was precipitated between phases. In a shaking funnel, the aqueous phase was separated off and the residue was again washed with water and then shaken thoroughly with 200 ml of petroleum ether. The precipitate was filtered off under suction and washed with petroleum ether. 6.5 g of the title compound of melting point 267°-277° C. were obtained in this manner.

후처리

  1. temperatureAfter cooling
  2. additionwere added
  3. customA solid was precipitated between phases
  4. customIn a shaking funnel, the aqueous phase was separated off
  5. washthe residue was again washed with water
  6. stirringshaken thoroughly with 200 ml of petroleum ether
  7. filtrationThe precipitate was filtered off under suction
  8. washwashed with petroleum ether

출처 및 근거

ORD 기록
ord-5db870c3a531410889b630b942b2bf38
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05061705

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