Dimethyl Sulfate → HCID 22452645, compound
Reaction equation
[OH:1][C:2]1[CH:3]=[C:4]([C:12]([OH:14])=[O:13])[C:5]2[CH2:6][CH2:7][CH2:8][CH2:9][C:10]=2[CH:11]=1.[OH-].[Na+].[CH3:17]OS(OC)(=O)=O>>[CH3:17][O:1][C:2]1[CH:3]=[C:4]([C:12]([OH:14])=[O:13])[C:5]2[CH2:6][CH2:7][CH2:8][CH2:9][C:10]=2[CH:11]=1Participants
4
Procedure
A mixture of 0.02 mole of 3-hydroxy-5,6,7,8-tetrahydronaphthalene-1-carboxylic acid, and 40 ml. of 2 N sodium hydroxide solution is treated with 0.04 mole of dimethylsulfate over a 5 minutes period, and the mixture is stirred for 24 hours. The mixture is washed with 3 × 50 ml. of ether and acidified with dilute hydrochloric acid. The precipitate is collected, washed with water, dried at room temperature and 100μ pressure and recrystallized from cyclohexane.
Workup
- washThe mixture is washed with 3 × 50 ml
- customThe precipitate is collected
- washwashed with water
- customdried at room temperature
- custom100μ pressure and recrystallized from cyclohexane
Sources & evidence
- ORD record
- ord-be87bbe540cf4fb5b9c31419c109741a
- Source dataset
- uspto-grants-1977_03
- Patent number
- US04011326
Reaction notes
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