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Methyl chloroformate → HCID 70414805、化合物

HRID 579759
ノート
印刷プレビュー

反応式

HRID 579759 の反応式
[H-].[Na+].[CH3:3][C:4]1[N:5]([CH2:9][CH:10]2[C:22](=[O:23])[C:21]3[C:20]4[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=4)[NH:14][C:13]=3[CH2:12][CH2:11]2)[CH:6]=[CH:7][N:8]=1.Cl[C:25]([O:27][CH3:28])=[O:26].C(=O)([O-])[O-].[Na+].[Na+].[C:35]([OH:42])(=[O:41])/[CH:36]=[CH:37]\[C:38]([OH:40])=[O:39]>CN(C)C=O.C(O)C>[C:35]([OH:42])(=[O:41])/[CH:36]=[CH:37]\[C:38]([OH:40])=[O:39].[CH3:28][O:27][C:25]([N:14]1[C:13]2[CH2:12][CH2:11][CH:10]([CH2:9][N:5]3[CH:6]=[CH:7][N:8]=[C:4]3[CH3:3])[C:22](=[O:23])[C:21]=2[C:20]2[C:15]1=[CH:16][CH:17]=[CH:18][CH:19]=2)=[O:26]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 6586Methyl chloroformateHCID 10340Sodium CarbonateHCID 24758Sodium hydrideHCID 444266Maleic AcidHCID 108912241,2,3,9-Tetrahydro-3-[(2-methyl-1H-imidazol-1-yl)methyl]-4H-carbazol-4-one

生成物 1

HCID 70414805HCID 70414805、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒2 回
HCID 6228Dimethylformamide溶媒

実験手順

Sodium hydride (0.075 g) was added to a solution of 1,2,3,9-tetrahydro-3-[(2-methyl-1H-imidazol-1-yl)methyl]-4H-carbazol-4-one (0.7 g) in dimethylformamide (10 ml) and the mixture was stirred at room temperature for 30 min. Methyl chloroformate (0.3 ml) was added and stirring continued at room temperature for 4 h. The resulting solution was basified with sodium carbonate (100 ml) filtered, and the filtrate was extracted with ethyl acetate (2×50 ml). The combined organic extracts and solid were washed with water (3×50 ml), dried (Na2SO4) and evaporated in vacuo to give a solid. Purification by flash chromatography (A) gave a solid, which was dissolved in ethanol (5 ml) and added to a solution of maleic acid (0.018 g) in ethanol (5 ml) to give the title compound (0.07 g) m.p. 91°-92°.

後処理

  1. stirringstirring
  2. waitcontinued at room temperature for 4 h
  3. filtrationfiltered
  4. extractionthe filtrate was extracted with ethyl acetate (2×50 ml)
  5. washThe combined organic extracts and solid were washed with water (3×50 ml)
  6. dry with materialdried (Na2SO4)
  7. customevaporated in vacuo
  8. customto give a solid
  9. customPurification by flash chromatography (A)
  10. customgave a solid, which

出典と根拠

ORDレコード
ord-6a7c0845b6894197b0a641754889d432
出典データセット
uspto-grants-1988_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04749718

反応ノート

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