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Dimethylformamide → HCID 68129031, 화합물

HRID 1077048
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HRID 1077048 반응식
[CH2:1]1[C:11]2[N:10]3[C:12]4[CH:21]=[CH:20][N:19]=[CH:18][C:13]=4[C:14]4[CH2:15][CH2:16][CH:17]=[C:8]([C:9]=43)[CH:7]=[CH:6][C:5]=2[CH2:4][CH2:3][CH2:2]1.[Cl:22][CH:23]([CH:25]1[CH2:27][CH2:26]1)[CH3:24].C(=O)(O)[O-].[Na+].CN(C)C=O>O>[ClH:22].[CH:25]1([CH:23]([CH:3]2[CH2:4][C:5]3[CH:6]=[CH:7][C:8]4[C:9]5[N:10]([C:12]6[CH:21]=[CH:20][N:19]=[CH:18][C:13]=6[C:14]=5[CH2:15][CH2:16][CH:17]=4)[C:11]=3[CH2:1][CH2:2]2)[CH3:24])[CH2:27][CH2:26]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 516892Sodium BicarbonateHCID 12627052(1-chloroethyl)cyclopropaneHCID 67838308HCID 67838308, 화합물

생성물 1

HCID 68129031HCID 68129031, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 5.5 g. of the product of Example 1, 2.3 g. of (1-chloroethyl)cyclopropane and 3.0 g. of sodium bicarbonate in 100 ml. of dimethylformamide is heated to 70°, with continued stirring, overnight, and the reaction mixture is then poured into water and extracted with ether. The extract is dried, evaporated to dryness, and the residue is dissolved in benzene and chromatographed. The eluate is then evaporated to dryness, the residue dissolved in absolute alcohol, treated with alcoholic hydrogen chloride, stripped down to dryness, and the glassy residue triturated with acetone to yield white crystals of the title compound, m.p. 249°-252°.

후처리

  1. additionA mixture of 5.5 g
  2. extractionextracted with ether
  3. customThe extract is dried
  4. customevaporated to dryness
  5. dissolutionthe residue is dissolved in benzene
  6. customchromatographed
  7. customThe eluate is then evaporated to dryness
  8. dissolutionthe residue dissolved in absolute alcohol
  9. additiontreated with alcoholic hydrogen chloride
  10. customthe glassy residue triturated with acetone

출처 및 근거

ORD 기록
ord-0e5a5076366a41d0a24425f37933fbb1
출처 데이터셋
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03959300

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