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Ethanol → HCID 13656010, 화합물

HRID 745899
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HRID 745899 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

HCID 13656010HCID 13656010, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-83430d2080774b3f8ba143fafc677b13
출처 데이터셋
uspto-grants-1986_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04602006

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