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Hydrochloric Acid → HCID 14343905, 화합물

HRID 35756
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HRID 35756 반응식
[H-].[Li+].[Al+3].[H-].[H-].[H-].Cl[CH2:8][CH2:9][C@H:10]1[C:19]([CH3:21])([CH3:20])[C:18]2[C:13](=[CH:14][CH:15]=[C:16]([CH3:22])[CH:17]=2)[C:12]([CH3:24])([CH3:23])[CH2:11]1.Cl>O1CCCC1>[CH2:9]([C@H:10]1[C:19]([CH3:21])([CH3:20])[C:18]2[C:13](=[CH:14][CH:15]=[C:16]([CH3:22])[CH:17]=2)[C:12]([CH3:23])([CH3:24])[CH2:11]1)[CH3:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14343902HCID 14343902, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 14343905HCID 14343905, 화합물수율 95.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a suspension of aluminum lithium hydride (6.5 g; 0.171 mol) in tetrahydrofuran (100 ml), a solution of (S)-3-(2-chloroethyl)-1,1,4,4,6-pentamethyl-1,2,3,4-tetrahydronaphthalene ([α]546 --33.4° (C=1.17 in ethanol)) (44.8 g; 0.169 mol) in tetrahydrofuran was dropwise added thereto. The resultant mixture was heated with reflux for 12 hours and then cooled. The cooled mixture was treated with dilute hydrochloric acid and extracted with n-hexane. The extract was washed with saturated sodium chloride solution, dried over anhydrous sodium sulfate and concentrated to give (R)-3-ethyl-1,1,4,4,6-pentamethyl-1,2,3,4-tetrahydronaphthalene (37.0 g; 0.161 mol; 94%). B.P., 79°-80° C./0.15 mmHg. [α]546 +2.2° (C=0.95 in ethanol).

후처리

  1. temperaturewith reflux for 12 hours
  2. temperaturecooled
  3. extractionextracted with n-hexane
  4. washThe extract was washed with saturated sodium chloride solution
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-188bc9bc7f564649b830b4a164b7c109
출처 데이터셋
uspto-grants-1988_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04767882

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