Claims
- 1. In the process for the production of 2-nitrobutylmorpholine from 1-nitropropane, morpholine and formaldehyde in about a 1.05-1.2:1.01:1 molar ratio the improvement comprising the steps of (a) mixing 1-nitropropane, and morpholine, (b) heating the mixture to about 55.degree.-60.degree. C., (c) then adding formaldehyde over about a 3-4 hour period, (d) holding the mixture at about 55.degree.-60.degree. C. for about a 2-3 hour period to make a total addition/holding period of at least six hours, (e) cooling the reaction mixture to form a two-phase oil-aqueous system, (f) collecting and discarding the water (upper) layer and (g) concentrating the oil layer to 2-nitrobutylmorpholine by removing excess water and 1-nitropropane.
- 2. The process of claim 1 wherein the formaldehyde is added over about a 3 hour period or more.
- 3. The process of claim 1 wherein said concentrating of the oil layer is performed by steam sparging.
- 4. The process of claim 1 wherein said concentrating of the oil layer is performed by extraction with water.
- 5. The process of claim 1 wherein said formaldehyde is added over a four-hour period and said mixture is held at 55.degree.-60.degree. C. for a two-hour period.
Parent Case Info
This is a continuation of copending application Ser. No. 741,175, filed Nov. 12, 1976.
Continuations (1)
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Number |
Date |
Country |
Parent |
741175 |
Nov 1976 |
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