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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Water → Naphthalene, 1,2,3,4-tetrahydro-1-methylene-

HRID 366380
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HRID 366380 반응식
[I-].[CH3:2][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[CH2:22]1[CH2:32][C:30](=O)[C:29]2[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=2)[CH2:23]1.O>C1COCC1>[CH2:2]=[C:30]1[C:29]2[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=2)[CH2:23][CH2:22][CH2:32]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 107241-TetraloneHCID 638159Methyltriphenylphosphonium iodide

생성물 1

HCID 141173Naphthalene, 1,2,3,4-tetrahydro-1-methylene-

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

N-Butyl lithium (Aldrich) (47 cm3, 74.8 mmol, 1.6 M solution in hexane) was added dropwise to a solution of methyl triphenylphosphonium iodide (Aldrich) (27.65 g, 68 mmol) in dry THF (150 cm3), under nitrogen at 0° C. α-Tetralone (Aldrich) (10 g, 68 mmol) in dry THF (100 cm3 was then added dropwise and the mixture stirred for 17 hours at room temperature. The reaction mixture was then added to water and extracted with ethyl acetate. The combined extracts were then dried (Na2SO4), filtered and concentrated in vacuo. Purification was by column chromatography on a neutralised silica column (Et3N) (Eluant: Pet. Ether 40-60° C.) produced a colourless mobile oil.

후처리

  1. additionwas then added dropwise
  2. extractionextracted with ethyl acetate
  3. dry with materialThe combined extracts were then dried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customPurification
  7. customwas by column chromatography on a neutralised silica column (Et3N) (Eluant: Pet. Ether 40-60° C.)
  8. customproduced a colourless mobile oil

출처 및 근거

ORD 기록
ord-64f9ec1362ec4bfbbaa76aa8642de618
출처 데이터셋
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06130228

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