2-Mercaptoethanol → HCID 512860, compound

HRID 1016525Notes

Reaction equation

HRID 1016525 reaction equation
[CH2:1]([N:10]1[C:15](=[O:16])[CH:14]=[C:12]([CH3:13])[C:11]1=[O:17])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH3:9].C(N(CC)CC)C.[SH:25][CH2:26][CH2:27][OH:28]>CN(C)C=O.C(OCC)(=O)C>[OH:28][CH2:27][CH2:26][S:25][C:12]1([CH3:13])[CH2:14][C:15](=[O:16])[N:10]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH3:9])[C:11]1=[O:17]

Participants

6

Reactant 3

HCID 15672-MercaptoethanolHCID 8471TriethylamineHCID 512824HCID 512824, compound

Product 1

HCID 512860HCID 512860, compound

Reagents, catalysts & solvents 2

HCID 6228DimethylformamideSolventHCID 8857Ethyl AcetateSolvent

Procedure

A solution of N-nonyl citraconimide (0.5 mM) prepared as described in Example 5 above in dimethylformamide (10 ml) was treated with triethylamine (0.5 mM) and then 2-mercaptoethanol (0.5 mM) was added dropwise. The progress of the reaction was monitored by thin layer chromatography and when the starting material could no longer be detected the reaction mixture was concentrated in vacuo. The residue obtained was dissolved in ethyl acetate, washed with water and dried over sodium sulfate. Purification by chromatography yielded the desired product.

Workup

  1. concentrationwas concentrated in vacuo
  2. customThe residue obtained
  3. washwashed with water
  4. dry with materialdried over sodium sulfate
  5. customPurification by chromatography

Sources & evidence

ORD record
ord-3ebbc23997294926ab078588017b3ab7
Source dataset
uspto-grants-2002_11
Patent number
US06476053B1

Reaction notes

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