Water → HCID 21285440, compound

HRID 2231719Notes

Reaction equation

HRID 2231719 reaction equation
[CH3:1][C:2]1(O)[C:10]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=2[N:4]2[CH2:11][CH2:12][CH2:13][N:14]=[C:3]12.S(=O)(=O)(O)O.O.C(=O)(O)[O-:23].[Na+].[C:27](#[N:29])[CH3:28]>CS(O)(=O)=O>[C:27]([NH:29][C:2]1([CH3:1])[C:10]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=2[N:4]2[CH2:11][CH2:12][CH2:13][N:14]=[C:3]12)(=[O:23])[CH3:28]

Participants

7

Reactant 5

HCID 962WaterHCID 1118Sulfuric AcidHCID 6342AcetonitrileHCID 516892Sodium BicarbonateHCID 54371730HCID 54371730, compound

Product 1

HCID 21285440HCID 21285440, compound

Reagents, catalysts & solvents 1

HCID 6395Methanesulfonic AcidCatalyst

Procedure

A solution of 2,3,4,10-tetrahydro-10-methylpyrimido [1,2-a]indol-10-ol (0.444 g) in acetonitrile (4 ml) and methanesulphonic acid (10 drops) was adde dropwise over 5 min to stirred sulphuric acid 98% w/w (2.5 ml) at 50°-60°. After 2.5h, the solution was poured into water (100 ml), basified with sat. aqueous sodium bicarbonate, and extracted with chloroform (3×100 ml). The extracts were washed with water (200 ml), dried (MgSO4), and evaporated in vacuo to give the title compound as the free base (0.07 g).

Workup

  1. extractionextracted with chloroform (3×100 ml)
  2. washThe extracts were washed with water (200 ml)
  3. dry with materialdried (MgSO4)
  4. customevaporated in vacuo

Sources & evidence

ORD record
ord-a750fa1b270d4b248670495ace780109
Source dataset
uspto-grants-1988_11
Patent number
US04783455

Reaction notes

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