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Potassium Carbonate → FR 110302

HRID 1089242
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HRID 1089242 반응식
[CH2:1]([C:5]1([CH2:17][CH2:18][CH2:19][CH3:20])[CH2:14][CH2:13][C:12]2[C:7](=[CH:8][CH:9]=[CH:10][C:11]=2[OH:15])[CH:6]1[OH:16])[CH2:2][CH2:3][CH3:4].Cl[CH2:22][C:23]1[CH:32]=[CH:31][C:30]2[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=2)[N:24]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O.[Cl-].[Na+].O>[CH2:1]([C:5]1([CH2:17][CH2:18][CH2:19][CH3:20])[CH2:14][CH2:13][C:12]2[C:7](=[CH:8][CH:9]=[CH:10][C:11]=2[O:15][CH2:22][C:23]2[CH:32]=[CH:31][C:30]3[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=3)[N:24]=2)[CH:6]1[OH:16])[CH2:2][CH2:3][CH3:4]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 203942-(Chloromethyl)quinolineHCID 105166192,2-Dibutyl-5-hydroxy-1,2,3,4-tetrahydro-1-naphthol

생성물 1

HCID 164102FR 110302수율 77.7%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 57417360
Sodium chloride; water
용매

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온도
70 °C

실험 절차

A mixture of (+)-2,2-dibutyl-5-hydroxy-1,2,3,4-tetrahydro-1-naphtol(138mg), 2-chloromethylquinoline(89 mg) and potassium carbonate(138 mg) in N,N-dimethylformamide(1 ml) was stirred at 70° C. for 3 hours. The cooled mixture was poured into brine(10 ml). The separated oil was extracted with brine(5 ml×3). The combined organic layers were washed with brine(5 ml), dried over magnesium sulfate and concentrated in vacuo. The residue was purified by columnchromatography on silica gel(elution by 15% ethyl acetate in hexane) to give a pale yellow syrup. The residual syrup was crystallized from methanol to yield (+)-2,2-dibutyl-5-(2-quinolylmethoxy)-1,2,3,4-tetrahydro-1naphtol(162 mg) as white solid.

후처리

  1. extractionThe separated oil was extracted with brine(5 ml×3)
  2. washThe combined organic layers were washed with brine(5 ml)
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by columnchromatography on silica gel(elution by 15% ethyl acetate in hexane)
  6. customto give a pale yellow syrup
  7. customThe residual syrup was crystallized from methanol

출처 및 근거

ORD 기록
ord-b6e24b56b23f4244b272a4042e246323
출처 데이터셋
uspto-grants-1990_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04965274

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