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

HRID 260417

反応式

HRID 260417 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8471Triethylamine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e83fd7405009452894335135ffaf77bf
出典データセット
uspto-grants-1996_06
特許番号
US05527862

関連ノート

読み込み中…