Chlorotrimethylsilane → 3,3'-Bis(trimethylsiloxy)-4,4'-bis(trimethylsilylamino)biphenyl

HRID 260417

반응식

HRID 260417 반응식
[OH:1][C:2]1[CH:3]=[C:4]([C:9]2[CH:14]=[CH:13][C:12]([NH2:15])=[C:11]([OH:16])[CH:10]=2)[CH:5]=[CH:6][C:7]=1[NH2:8].COC1C=C(C2C=CC(N)=C(OC)C=2)C=CC=1N.I.[CH3:36][Si:37]([CH3:40])([CH3:39])Cl>O1CCCC1.C(N(CC)CC)C>[CH3:36][Si:37]([CH3:40])([CH3:39])[O:1][C:2]1[CH:3]=[C:4]([C:9]2[CH:14]=[CH:13][C:12]([NH:15][Si:37]([CH3:40])([CH3:39])[CH3:36])=[C:11]([O:16][Si:37]([CH3:40])([CH3:39])[CH3:36])[CH:10]=2)[CH:5]=[CH:6][C:7]=1[NH:8][Si:37]([CH3:40])([CH3:39])[CH3:36]

참가 물질

7

반응물 4

HCID 6397ChlorotrimethylsilaneHCID 8411DianisidineHCID 169183,3'-DihydroxybenzidineHCID 24841Hydrogen iodide

생성물 1

HCID 111563923,3'-Bis(trimethylsiloxy)-4,4'-bis(trimethylsilylamino)biphenyl

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8471Triethylamine용매

실험 절차

0.540 g of 3,3'-dihydroxy-4,4'-diaminobiphenyl (synthesized from 3,3'-dimethoxy-4,4'-diaminobiphenyl using hydrogen iodide by the known method) and 1.52 g of triethylamine were dissolved in 16 mL of dry tetrahydrofuran. 1.63 g of trimethylchlorosilane was then added dropwise followed by heating under reflux for 72 hours. Operating in an argon atmosphere, the salt was filtered off and the solvent, etc., was removed under reduced pressure to yield 3,3'-bis(trimethylsiloxy)-4,4'-bis(trimethylsilylamino)biphenyl.

후처리

  1. temperatureby heating
  2. temperatureunder reflux for 72 hours
  3. filtrationOperating in an argon atmosphere, the salt was filtered off
  4. customthe solvent, etc., was removed under reduced pressure

출처 및 근거

ORD 기록
ord-e83fd7405009452894335135ffaf77bf
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05527862

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