Pyridine → 2-Mesyloxy-1,2,3,4-tetrahydro-tribenzo(b,d,f)-oxepine

HRID 1703975Notes

Reaction equation

HRID 1703975 reaction equation
[OH:1][CH:2]1[CH2:20][CH2:19][C:5]2[C:6]3[CH:18]=[CH:17][CH:16]=[CH:15][C:7]=3[O:8][C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=3[C:4]=2[CH2:3]1.N1C=CC=CC=1.[CH3:27][S:28](Cl)(=[O:30])=[O:29]>O>[S:28]([O:1][CH:2]1[CH2:20][CH2:19][C:5]2[C:6]3[CH:18]=[CH:17][CH:16]=[CH:15][C:7]=3[O:8][C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=3[C:4]=2[CH2:3]1)([CH3:27])(=[O:30])=[O:29]

Participants

5

Reactant 3

HCID 1049PyridineHCID 31297Methanesulfonyl chlorideHCID 22760978HCID 22760978, compound

Product 1

HCID 227609192-Mesyloxy-1,2,3,4-tetrahydro-tribenzo(b,d,f)-oxepine

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
0 °C

Procedure

6.2 g of 2-hydroxy-1,2,3,4-tetrahydro-tribenzo(b,d,f)-oxepine are added to a mixture of 16.8 ml of pyridine and methane sulphonylchloride, after which the mixture is stirred for 2 hours at 0° C. and then another 2 hours at room temperature. After that the mixture is poured out into water and then extracted with ether. The ether layers are dried and evaporated to dryness.

Workup

  1. customanother 2 hours
  2. customat room temperature
  3. extractionextracted with ether
  4. dry with materialThe ether layers are dried
  5. customevaporated to dryness

Sources & evidence

ORD record
ord-84d491e09dc946c4b3fccdc82c3d3b6d
Source dataset
uspto-grants-1978_11
Patent number
US04125718

Reaction notes

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