Methanol → Bis(trihexylsiloxy)silicon 2,3-naph- thalocyanine

HRID 1589054ノート

反応式

HRID 1589054 の反応式
[CH2:1]([Si:7]([CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH3:20])([CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14])[OH:8])[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].C[O-].[Na+].[CH:24]1[CH:29]=[C:28]2[C:30]3[N-:63][C:62]([C:27]2=[CH:26][CH:25]=1)=[N:61][C:59]1=[N:60][C:52]([C:53]2[C:58]1=[CH:57][CH:56]=[CH:55][CH:54]=2)=[N:51][C:49]1=[N:50][C:42]([C:43]2[C:48]1=[CH:47][CH:46]=[CH:45][CH:44]=2)=[N:41][C:39]1[N-:40][C:32](=[C:33]2[C:38]=1[CH:37]=[CH:36][CH:35]=[CH:34]2)[N:31]=3.[Si+4:64].[Cl-].[Cl-].CO>C(O)C>[CH3:20][CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][Si:7]([O-:8])([CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14])[CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].[CH3:20][CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][Si:7]([O-:8])([CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14])[CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].[CH:2]1[CH:1]=[C:35]2[C:36]([CH:37]=[C:38]3[C:39]4[N-:40][C:32](=[N:31][C:30]5[N-:63][C:62]([N:61]=[C:59]6[N:60]=[C:52]([N:51]=[C:49]7[N:50]=[C:42]([N:41]=4)[C:43]4[C:48]7=[CH:47][C:46]7[C:45]([CH:44]=4)=[CH:17][CH:18]=[CH:19][CH:20]=7)[C:53]4[C:58]6=[CH:57][C:56]6[C:55]([CH:54]=4)=[CH:9][CH:10]=[CH:11][CH:12]=6)=[C:27]4[C:28]=5[CH:29]=[C:24]5[C:25](=[CH:26]4)[CH:15]=[CH:16][CH:17]=[CH:18]5)[C:33]3=[CH:34]2)=[CH:4][CH:3]=1.[Si+4:64]

参加物

6

反応物 4

HCID 887MethanolHCID 163603TRIHEXYLSILANOLHCID 10942334Sodium MethoxideHCID 178478905HCID 178478905、化合物2 回

生成物 1

HCID 163602Bis(trihexylsiloxy)silicon 2,3-naph- thalocyanine収率 79%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of tri-n-hexylsilanol (14.9 g), sodium methoxide (2.67 g) and absolute ethanol (50 ml) was reduced to an oil under vacuum. This oil was added to a mixture of dichlorosilicon phthalocyanine (Formula 9, from Aldrich Chemical CO., Milwaukee, Wis., 15.10 g) and distilled, dry 1,2,4-trimethyl-benzene (70 ml). The resulting suspension was refluxed for 1 hr and was filtered hot using Whatman #54 filter paper. The filtrate was allowed to cool (12 hr) and was diluted with methanol (350 mol). The precipitated product of Formula 10 was isolated by filtration, washed with methanol (100 ml) and vacuum dried at room temperature overnight, (22.06 g, 79% yield) m.pt. 175° C.; IR (Nujol) 1525 (s), 1325 (s), 1125(s), 1080 (s), 1038 (s, Si--O--Si), 725 (s) cm-1.

後処理

  1. distillationdistilled
  2. temperatureThe resulting suspension was refluxed for 1 hr
  3. filtrationwas filtered hot
  4. filtrationfilter paper
  5. temperatureto cool (12 hr)

出典と根拠

ORDレコード
ord-4dcde6f944384596b06f072e41fafb48
出典データセット
uspto-grants-1993_06
特許番号
US05224196

反応ノート

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