Gamma-Butyrolactone → Gamma-Butyrolactone
Reaction equation
[H][H].[C:3]1(=[O:8])[O:7][CH2:6][CH2:5][CH2:4]1>>[C:3]1(=[O:8])[O:7][CH2:6][CH2:5][CH2:4]1.[CH:3]([OH:8])([OH:7])[CH2:4][CH2:5][CH3:6]Participants
Conditions
- Temperature
- 160 °C
Procedure
A stainless steel tubular reaction with an O.D. of 1 inch and I.D. 0.93 inches was packed with 70 ml (27 g.) of the catalyst from Example 1 to provide a 7 inch bed length. The catalyst was reduced over a six hour period 150°-300° C. using hydrogen in nitrogen in increasing concentration of from about 3% to about 10% H2. The hydrogen mixture was introduced intermittently until there was little exotherm, after which the hydrogen concentration was increased to 100%. A feed of γ-Butyrolactone was pumped to a vaporizer from which the vapor was carried by a hydrogen stream to the reaction. The ratio of hydrogen to butyrolactone feed (99% pure) was 150:1. The reactor was maintained at 160° C. temperature, 600 psig. pressure and an LHSV of 0.05 (g. of feed/hour/volume of catalyst). The product vapors were collected and condensed. A conversion of 90% butyrolactone with 95% selectivity to butanediol was obtained.
Workup
- customto provide a 7 inch bed length
- temperaturein increasing concentration of from about 3% to about 10% H2
- concentrationafter which the hydrogen concentration
- temperaturewas increased to 100%
- customwas carried by a hydrogen stream to the reaction
- customThe product vapors were collected
- customcondensed
Sources & evidence
- ORD record
- ord-ccf40e02971e44cfab176528c40399d4
- Source dataset
- uspto-grants-1989_01
- Patent number
- US04797382
Reaction notes
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