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Hexane → HCID 71245442, 화합물

HRID 575501
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HRID 575501 반응식
[CH3:1][O:2][C:3]1[C:18]2[C:14]3[S:15][CH:16]=[CH:17][C:13]=3[CH:12]=[C:11]([O:19][CH3:20])[C:10]=2[C:6]2[S:7][CH:8]=[CH:9][C:5]=2[CH:4]=1.[C:21](Cl)(=[O:33])[CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32].[Cl-].[Cl-].[Cl-].[Al+3].CCCCCC>ClCCl>[CH3:20][O:19][C:11]1[C:10]2[C:6]3[S:7][C:8]([C:21](=[O:33])[CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32])=[CH:9][C:5]=3[CH:4]=[C:3]([O:2][CH3:1])[C:18]=2[C:14]2[S:15][CH:16]=[CH:17][C:13]=2[CH:12]=1
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참가 물질

6

반응물 4

HCID 8058HexaneHCID 8166Dodecanoyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 712456764,9-Dimethoxynaphtho[1,2-b:5,6-b']dithiophene

생성물 1

HCID 71245442HCID 71245442, 화합물수율 54%

시약·촉매·용매 1

HCID 6344Dichloromethane
용매

실험 절차

4,9-Dimethoxynaphtho[1,2-b:5,6-b′]dithiophene (0.90 g, 3.0 mmol) was solubilized in anhydrous dichloromethane (20 mL). Dodecanoyl chloride (0.765 g, 3.5 mmol) was then added and stirring was continued for 10 minutes at this temperature. Aluminum trichloride (0.465 g, 3.5 mmol) was then added in 3 portions. The mixture was stirred overnight at room temperature. The mixture was cooled in ice water and extracted with chloroform (200 mL) and washed with water (100 mL) and brine (50 mL). After the solvent was removed, the residual was purified using a silica column with dichloromethane:hexane (1/3) to give compound 1-(4,9-dimethoxynaphtho[1,2-b:5,6-b′]dithiophen-2-yl)dodecan-1-one as a pale yellow solid (0.78 g, ˜54% yield). 1H NMR (500 MHz, CDCl3): δ 8.72 (s, 1H), 7.69 (d, J=5.5 Hz, 1H), 7.50 (m, 2H), 7.42 (s, 1H), 4.24 (s, 3H), 4.22 (s, 3H) 3.07. (t, J=7.0 Hz, 2H), 1.83 (m, 2H), 1.39 (m, 18H); 0.88 (m, J=6.0 Hz, 3H).

후처리

  1. stirringThe mixture was stirred overnight at room temperature
  2. extractionextracted with chloroform (200 mL)
  3. washwashed with water (100 mL) and brine (50 mL)
  4. customAfter the solvent was removed
  5. customthe residual was purified

출처 및 근거

ORD 기록
ord-b3c7173ef1534b90887d0c10e82ba97d
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09035004B2

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