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Dimethylformamide → HCID 68129031、化合物

HRID 1077048
ノート
印刷プレビュー

反応式

HRID 1077048 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 516892Sodium BicarbonateHCID 12627052(1-chloroethyl)cyclopropaneHCID 67838308HCID 67838308、化合物

生成物 1

HCID 68129031HCID 68129031、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-0e5a5076366a41d0a24425f37933fbb1
出典データセット
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03959300

反応ノート

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