Water → HCID 136365464, compound

HRID 1106381Notes

Reaction equation

HRID 1106381 reaction equation
C[O:2][Si:3][O:4]C.[CH:6]1[CH:7]=[CH:8][C:9]2[C:10](=[C:12]3[N:44]=[C:43]4[N:45]=[C:36]([C:37]5[CH:38]=[CH:39][CH:40]=[CH:41][C:42]=54)[N:35]=[C:33]4[NH:34][C:26]([C:27]5[CH:28]=[CH:29][CH:30]=[CH:31][C:32]=54)=[N:25][C:23]4=[N:24][C:16]([C:17]5[CH:18]=[CH:19][CH:20]=[CH:21][C:22]=54)=[N:15][C:14]=2[NH:13]3)[CH:11]=1.O>CN1CCCC1=O>[OH:2][Si:3][OH:4].[CH:7]1[CH:6]=[CH:11][C:10]2[C:9](=[C:14]3[N:15]=[C:16]4[N:24]=[C:23]([C:22]5[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=54)[N:25]=[C:26]4[NH:34][C:33]([C:32]5[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=54)=[N:35][C:36]4=[N:45][C:43]([C:42]5[CH:41]=[CH:40][CH:39]=[CH:38][C:37]=54)=[N:44][C:12]=2[NH:13]3)[CH:8]=1

Participants

4

Reactant 2

HCID 962WaterHCID 136473082HCID 136473082, compound

Product 1

HCID 136365464HCID 136365464, compoundYield 83.9%

Reagents, catalysts & solvents 1

HCID 13387N-methyl-2-pyrrolidoneSolvent

Procedure

10 g of dimethoxysilicon phthalocyanine synthesized in Synthesis Example 2 was added to 5 g of water and 95 g of N-methylpyrrolidone (95% NMP aqueous solution) and reacted at 148° C. for 3 hours. The reaction product was thermally filtrated and washed with NMP and acetone in the order named. After the product was stirred in 100 ml of acetone at room temperature, crystals were separated by filtration and dried to obtain 8.0 g of dihydroxysilicon phthalocyanine. When structural analysis was carried out by mass spectral (negative measurement) and IR (KBr method) methods, the same spectrum as that of Example 1 was obtained. Therefore, it was confirmed that the product was dihydroxysilicon phthalocyanine. When the structural analysis of the obtained dihydroxysilicon phthalocyanine was carried out in accordance with the method of Itoh, it was found to be monoclinic and have lattice constants a=12.79Å, b=14.61Å, c=6.79Å and β=94.4°. According to the X-ray spectrum (FIG. 10), it is a dihydroxysilicon phthalocyanine having the crystal form of the present invention and a main peak at a 2 θ of 9.2° and other peaks at 12.2, 14.0, 15.3, 19.7, 23.4 and 27.1°, respectively.

Workup

  1. customreacted at 148° C. for 3 hours
  2. filtrationThe reaction product was thermally filtrated
  3. washwashed with NMP and acetone in the order
  4. customcrystals were separated by filtration
  5. customdried

Sources & evidence

ORD record
ord-20c1d67bc4164e8faaf659a126a8693e
Source dataset
uspto-grants-2000_05
Patent number
US06057071

Reaction notes

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