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Ethanol → HCID 13656010、化合物

HRID 745899
ノート
印刷プレビュー

反応式

HRID 745899 の反応式
[CH3:1][Si:2]([CH3:12])([CH3:11])[C:3]#[C:4][CH2:5][CH2:6][CH2:7][C:8]([OH:10])=[O:9].[CH2:13](O)[CH3:14].N1C=CC=CC=1>O1CCCC1>[CH3:12][Si:2]([CH3:1])([CH3:11])[C:3]#[C:4][CH2:5][CH2:6][CH2:7][C:8]([O:10][CH2:13][CH3:14])=[O:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 702EthanolHCID 1049PyridineHCID 119900745-Hexynoic acid, 6-(trimethylsilyl)-

生成物 1

HCID 13656010HCID 13656010、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of 5.3 gm of 1,1-carbonyldiimidazole in 80 ml of dry tetrahydrofuran under argon, was added a solution of 5.03 gm of 6-trimethylsilyl-5-hexynoic acid in 15 ml of dry tetrahydrofuran. The mixture was stirred for 1 hour. Absolute ethanol (80 ml) and pyridine (1 ml) were then added, and the resulting mixture was stirred at room temperature for 48 hours. The solvent was evaporated and the residual oil was extracted with ether and 1.5% hydrochloric acid. The ethereal layer, which was washed with water and then dried, was evaporated to an oil. This material was purified by distillation, b.p. 70°-75° C. (0.6 mm Hg); IR: 2170, 1735 cm-1.

後処理

  1. stirringthe resulting mixture was stirred at room temperature for 48 hours
  2. customThe solvent was evaporated
  3. extractionthe residual oil was extracted with ether and 1.5% hydrochloric acid
  4. washThe ethereal layer, which was washed with water
  5. customdried
  6. customwas evaporated to an oil
  7. distillationThis material was purified by distillation, b.p. 70°-75° C. (0.6 mm Hg)

出典と根拠

ORDレコード
ord-83430d2080774b3f8ba143fafc677b13
出典データセット
uspto-grants-1986_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04602006

反応ノート

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