L-Selenocysteine → Bis(dimethyl-octadecyl-siloxy)germanium phthalocyanine

HRID 1379003ノート

反応式

HRID 1379003 の反応式
N[C@H:2]([C:5](O)=O)[CH2:3][SeH].[CH3:8][Si:9]([CH3:29])([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])Cl.[OH:30][Ge:31][OH:32].[CH:33]1[CH:34]=[CH:35][C:36]2[C:37](=[C:39]3[N:71]=[C:70]4[N:72]=[C:63]([C:64]5[CH:65]=[CH:66][CH:67]=[CH:68][C:69]=54)[N:62]=[C:60]4[NH:61][C:53]([C:54]5[CH:55]=[CH:56][CH:57]=[CH:58][C:59]=54)=[N:52][C:50]4=[N:51][C:43]([C:44]5[CH:45]=[CH:46][CH:47]=[CH:48][C:49]=54)=[N:42][C:41]=2[NH:40]3)[CH:38]=1>N1C=CC=CC=1>[CH3:8][Si:9]([CH3:29])([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])[O:30][Ge:31][O:32][Si:9]([CH2:3][CH2:2][CH2:5][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:70][CH2:69][CH2:68][CH2:67][CH2:66][CH2:65][CH2:64][CH3:63])([CH3:11])[CH3:8].[CH:34]1[CH:33]=[CH:38][C:37]2[C:36](=[C:41]3[N:42]=[C:43]4[N:51]=[C:50]([C:49]5[CH:48]=[CH:47][CH:46]=[CH:45][C:44]=54)[N:52]=[C:53]4[NH:61][C:60]([C:59]5[CH:58]=[CH:57][CH:56]=[CH:55][C:54]=54)=[N:62][C:63]4=[N:72][C:70]([C:69]5[CH:68]=[CH:67][CH:66]=[CH:65][C:64]=54)=[N:71][C:39]=2[NH:40]3)[CH:35]=1

参加物

5

反応物 3

HCID 25076L-SelenocysteineHCID 87738OctadecyldimethylchlorosilaneHCID 178526211HCID 178526211、化合物

生成物 1

HCID 137226509Bis(dimethyl-octadecyl-siloxy)germanium phthalocyanine

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

[In analogy to a procedure by Wheeler et. al., J. Am. Chem. Sec. 106, 7404 (1984)] 3.3 g (9.5 mmol) of dimethyl-octadecyl-chlorosilane and 0.5 g (0.8 mmol) of dihydroxygermanium-phthalocyanine in 50 ml of pyridine are stirred for 2 hours at 50°. The solution is cooled and filtered using a suction filter. The solvent is removed in vacuo, and 250 ml of hexane are added to the residue. The resulting precipitate is filtered off with suction and washed first with hexane, then in portions with 200 ml of acetone/water (1:1). The residue is dried overnight under a high vacuum, then extracted with toluene in a Soxhlet, freed of solvent and dried, yielding bis(dimethyl-octadecyl-siloxy)germanium-phthalocyanine; NMR (pyridine-d5): δ=9.8-9.9 (m, 8H); 8.3-8.5 (m,8H): aromatic H's; 0.75-1.46 (various m's); 0.45(m); -0.03 (m); -0.88 (m); -1.91 (m); -2.48 (m, 4×CH3 : silyl side chains) ppm.

後処理

  1. temperatureThe solution is cooled
  2. filtrationfiltered
  3. filtrationfilter
  4. customThe solvent is removed in vacuo, and 250 ml of hexane
  5. additionare added to the residue
  6. filtrationThe resulting precipitate is filtered off with suction
  7. washwashed first with hexane
  8. customThe residue is dried overnight under a high vacuum
  9. extractionextracted with toluene in a Soxhlet
  10. customdried

出典と根拠

ORDレコード
ord-19f8da6eee6249d78df90e7691d9d5d2
出典データセット
uspto-grants-1997_09
特許番号
US05670491

反応ノート

読み込み中…