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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Hydrochloric Acid → HCID 68603754, 화합물

HRID 1803002
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HRID 1803002 반응식
[Cl-].[Li+].Br[C:4]1[CH:9]=[C:8]([O:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16])[C:7]([I:17])=[CH:6][C:5]=1[O:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24].C1C2C(=CC=CC=2)C=CC=1.C([Mg]Cl)(C)C.BrC1SC(Br)=CC=1CCCCCC.Cl>C1COCC1>[CH2:19]([O:18][C:5]1[CH:6]=[C:7]([I:17])[C:8]([O:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16])=[CH:9][CH:4]=1)[CH2:20][CH2:21][CH2:22][CH2:23][CH3:24]
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참가 물질

8

반응물 6

HCID 313Hydrochloric AcidHCID 931Naphthalene2회HCID 433294Lithium ChlorideHCID 3936632Thiophene, 2,5-dibromo-3-hexyl-2회HCID 686032211-Bromo-2,5-bis(hexyloxy)-4-iodobenzene2회HCID 178418918HCID 178418918, 화합물2회

생성물 1

HCID 68603754
HCID 68603754, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매6회

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온도
0 °C

실험 절차

0.042 g (0.99 mmol) of anhydrous lithium chloride was put in a flask, and vacuum dried with heating the flask using a heat gun, followed by carrying out argon substitution and returning the temperature to room temperature. Thereto were added 0.483 g (1.00 mmol) of 1-bromo-2,5-dihexyloxy-4-iodobenzene and 0.0448 g (0.350 mmol) of naphthalene as an internal standard material, and the flask was again subjected to argon substitution. 5 mL of dried THF was added thereto, and 0.5 mL (1.0 mmol) of a solution of isopropylmagnesium chloride in THF (2.0 mol/l) was added, followed by stirring for 1 hour at 0° C. to Grignardize the 1-bromo-2,5-dihexyloxy-4-iodobenzene. Thereafter, 0.0105 g (0.0199 mmol, 2.0 mol %) of Ni(dppe)Cl2 suspended in 5 mL of THF was added, followed by stirring at room temperature for 30 minutes. In another egg-plant type flask were put 0.373 g (1.00 mmol) of 2,5-dibromo-3-hexylthiophene, 0.0329 g (0.257 mmol) of naphthalene, 5 mL of dried THF and 0.5 mL (1.0 mmol) of a solution of isopropylmagnesium chloride in THF (2.0 mol/l), and they were stirred at 0° C. for 1 hour to Grignardize 2,5-dibromo-3-hexylthiophene. A THF solution thereof was added to the reaction mixture, followed by stirring at room temperature for 10 minutes. After completion of the reaction, 5M HCl was added, followed by extraction with chloroform, and the organic layer was washed with water and then dried with anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain a block copolymer (Mn=16200, Mw/Mn=1.27) represented by the following formula. A block copolymer having a narrow molecular weight distribution was obtained by first polymerizing the Grignardized 2,5-dihexyloxy-4-iodobenzene greater in parameter of aromatic ring charge (−0.104), and then copolymerizing 2,5-dibromo-3-hexylthiophene (−0.116).

후처리

  1. customvacuum dried
  2. temperaturewith heating the flask
  3. customto room temperature
  4. additionwas added
  5. stirringby stirring at room temperature for 30 minutes
  6. customIn another egg-plant type flask were put
  7. stirringby stirring at room temperature for 10 minutes
  8. additionwas added
  9. extractionfollowed by extraction with chloroform
  10. washthe organic layer was washed with water
  11. dry with materialdried with anhydrous magnesium sulfate
  12. distillationThe solvent was distilled off under reduced pressure
  13. customto obtain a block copolymer (Mn=16200, Mw/Mn=1.27)

출처 및 근거

ORD 기록
ord-1753165a767142f5bd619e2c703b42fa
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08349997B2

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