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Tetraethyl [[1,1'-biphenyl]-4,4'-diylbis(methylene)]bis(phosphonate) → HCID 67430310、化合物

HRID 1660680
ノート
印刷プレビュー

反応式

HRID 1660680 の反応式
[CH3:1][C:2]([CH3:5])([O-])[CH3:3].[K+].[CH3:7][N:8]1[C:21]2[CH:20]=[CH:19][C:18]([CH:22]=O)=[CH:17][C:16]=2[S:15](=[O:25])(=[O:24])[C:14]2[C:9]1=[CH:10][CH:11]=[CH:12][CH:13]=2.C(OP([CH2:34][C:35]1[CH:40]=[CH:39][C:38]([C:41]2[CH:46]=[CH:45][C:44]([CH2:47]P(OCC)(OCC)=O)=[CH:43][CH:42]=2)=[CH:37][CH:36]=1)(=O)OCC)C>CS(C)=O.CN1CCCC1=O>[CH3:7][N:8]1[C:21]2[CH:20]=[CH:3][C:2]([CH:5]=[CH:47][C:44]3[CH:43]=[CH:42][C:41]([C:38]4[CH:37]=[CH:36][C:35]([CH:34]=[CH:22][C:18]5[CH:19]=[CH:20][C:21]6[N:8]([CH3:7])[C:9]7[C:14]([S:15](=[O:25])(=[O:24])[C:16]=6[CH:17]=5)=[CH:13][CH:12]=[CH:11][CH:10]=7)=[CH:40][CH:39]=4)=[CH:46][CH:45]=3)=[CH:1][C:16]=2[S:15](=[O:25])(=[O:24])[C:14]2[C:9]1=[CH:10][CH:11]=[CH:12][CH:13]=2
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 635132Tetraethyl [[1,1'-biphenyl]-4,4'-diylbis(methylene)]bis(phosphonate)HCID 23665647Potassium tert-butoxideHCID 86648277HCID 86648277、化合物

生成物 1

HCID 67430310HCID 67430310、化合物

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒
HCID 13387
N-methyl-2-pyrrolidone
溶媒

実験手順

1.02 g (9.05 mmol) of potassium tert-butoxide and then 2.20 g (8.05 mmol) of 10-methyl-5,5-dioxophenothiazine-3-carbaldehyde (Example 21) were added under nitrogen at room temperature with stirring to a solution of 1.82 g (4.00 mmol) of diethyl[4′-(diethoxyphosphorylmethyl)biphenyl-4-ylmethyl]phosphonate in 41 ml of dimethyl sulfoxide dried over molecular sieve. After stirring at room temperature for four hours, the reaction solution was diluted with 90 ml of methanol and stirred for a further 15 min. The precipitate was filtered off, washed with 220 ml of methanol and dried at 35° C. under reduced pressure. The crude product (2.50 g) was recrystallized in 58 ml of dimethyl sulfoxide. After solvent residues had been removed under high vacuum at 200° C., 1.64 g (59% of theory) of analytically pure yellow solid having a melting point of 360° C. were obtained, whose solution in N-methylpyrrolidone fluoresced at λ=460 nm.

後処理

  1. customdried over molecular sieve
  2. additionthe reaction solution was diluted with 90 ml of methanol
  3. stirringstirred for a further 15 min
  4. filtrationThe precipitate was filtered off
  5. washwashed with 220 ml of methanol
  6. customdried at 35° C. under reduced pressure
  7. customThe crude product (2.50 g) was recrystallized in 58 ml of dimethyl sulfoxide
  8. customAfter solvent residues had been removed under high vacuum at 200° C.
  9. customwere obtained

出典と根拠

ORDレコード
ord-bbaeea5cb6e64dccaa1f79ff8b0c353f
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08029919B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート