(4-(2,2-Dimethyl-1,3-dioxan-5-yl)methoxy-3,5-dimethylpyridin-2-yl)methanol monohydrate → HCID 178527752, compound

HRID 31717Notes

Reaction equation

HRID 31717 reaction equation
[Na].CC1C(C[S:23]([C:25]2[NH:29][C:28]3[CH:30]=[CH:31][CH:32]=[CH:33][C:27]=3[N:26]=2)=O)=NC=CC=1OCC1(C)OCC2(OCCO2)CO1.CC1(C)OCC(COC2C(C)=CN=[C:45]([CH2:50][OH:51])C=2C)CO1.O.CC1(C)OCC(COC2C(C)=CN=C(CO)C=2C)C[O:57]1>C1(C)C=CC=CC=1>[NH:29]1[C:28]2[CH:30]=[C:31]3[O:51][CH2:50][CH2:45][O:57][C:32]3=[CH:33][C:27]=2[N:26]=[C:25]1[SH:23]

Participants

5

Reactant 3

HCID 57445207(4-(2,2-Dimethyl-1,3-dioxan-5-yl)methoxy-3,5-dimethylpyridin-2-yl)methanol monohydrateHCID 57445208(4-((2,2-Dimethyl-1,3-dioxan-5-yl)methoxy)-3,5-dimethylpyridin-2-yl)methanolHCID 667765502-(((3-Methyl-4-((8-methyl-1,4,7,9-tetraoxaspiro[4.5]dec-8-yl)methoxy)pyridin-2-yl)methyl)sulfinyl)-1h-benzimidazole sodium salt

Product 1

HCID 178527752HCID 178527752, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

The same procedure as in the steps (5f) to (5h) was repeated using the (4-((2,2-dimethyl-1,3-dioxan-5-yl)methoxy)-3,5-dimethylpyridin-2-yl)methanol, which was obtained by subjecting (4-((2,2-dimethyl-1,3-dioxan-5-yl)methoxy)-3,5-dimethylpyridin-2-yl)methanol monohydrate obtained in the same manner as in Example 96(5) to azeotropic distillation with toluene, and 6,7-dihydro-1H-[1,4]dioxino[2′,3′:4,5]benzo[d]imidazole-2-thiol, to obtain the title compound (395 mg, total 61.7% yield) as a white solid.

Workup

  1. customwhich was obtained

Sources & evidence

ORD record
ord-5ec1c78016004ed2b9a8fee0f988b952
Source dataset
uspto-grants-2008_09
Patent number
US07425634B2

Reaction notes

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