4-(1,1,3,3,3-Pentamethy-disiloxanyl)-butanol → Cyano-(2,3-dihydro-5-methoxy-2-methyl-1H-inden-1-ylidene)acetic Acid-4-(1,1,3,3,3-pentamethy-disiloxanyl)-butyl Ester

HRID 2228347

反応式

HRID 2228347 の反応式
[CH3:1][Si:2]([CH2:9][CH2:10][CH2:11][CH2:12][OH:13])([CH3:8])[O:3][Si:4]([CH3:7])([CH3:6])[CH3:5].C(C(CCCC)C[O:18][C:19](=O)[C:20]([C:33]#[N:34])=[C:21]1[C:29]2[C:24](=[CH:25][C:26]([O:30][CH3:31])=[CH:27][CH:28]=2)[CH2:23][CH:22]1[CH3:32])C>>[CH3:8][Si:2]([CH2:9][CH2:10][CH2:11][CH2:12][O:13][C:19](=[O:18])[C:20]([C:33]#[N:34])=[C:21]1[C:29]2[C:24](=[CH:25][C:26]([O:30][CH3:31])=[CH:27][CH:28]=2)[CH2:23][CH:22]1[CH3:32])([CH3:1])[O:3][Si:4]([CH3:5])([CH3:7])[CH3:6]

参加物

3

反応物 2

HCID 108678254-(1,1,3,3,3-Pentamethy-disiloxanyl)-butanolHCID 69822365cyano-(2,3-dihydro-5-methoxy-2-methyl-1H-inden-1-ylidene)acetic acid 2-ethyl-hexyl ester

生成物 1

HCID 69822753Cyano-(2,3-dihydro-5-methoxy-2-methyl-1H-inden-1-ylidene)acetic Acid-4-(1,1,3,3,3-pentamethy-disiloxanyl)-butyl Ester収率 30%

実験手順

The reaction of Example 2b was repeated using 4-(1,1,3,3,3-pentamethy-disiloxanyl)-butanol (see above) instead of 3-(1,1,3,3,3-pentamethy-disiloxanyl)-propanol as well as the above cyano-(2,3-dihydro-5-methoxy-2-methyl-1H-inden-1-ylidene)acetic acid 2-ethyl-hexyl ester instead of the product of example 1. After 9 hours of reaction time, the product was concentrated and then treated for another 5 hours as set forth above with new 3-(1,1,3,3,3-pentamethy-disiloxanyl)-propanol. The mixture was then concentrated and chromatographed as before to yield 30% of a liquid material. UV 347 nm (ε=32′500). This product had the same solubility and photostability qualities as described in Example 2b.

後処理

  1. customThe reaction of Example 2b
  2. customAfter 9 hours of reaction time
  3. concentrationthe product was concentrated
  4. additiontreated for another 5 hours
  5. concentrationThe mixture was then concentrated
  6. customchromatographed as before

出典と根拠

ORDレコード
ord-602a27df2ef7431bb22d613590be57e5
出典データセット
uspto-grants-2002_07
特許番号
US06416746B1

関連ノート

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