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

HRID 1589054노트

반응식

HRID 1589054 반응식
[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]

참가 물질

6

반응물 4

HCID 887MethanolHCID 163603TRIHEXYLSILANOLHCID 10942334Sodium MethoxideHCID 178478905HCID 178478905, 화합물2회

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-4dcde6f944384596b06f072e41fafb48
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05224196

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