Acetic-formic anhydride → HCID 14126428, compound

HRID 568575Notes

Reaction equation

HRID 568575 reaction equation
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[NH:12][CH2:11][C:10]3[CH:13]=[CH:14][CH:15]=[CH:16][C:9]=3[S:8][C:7]=2[CH:17]=1.[C:18](OC=O)(=[O:20])C>O1CCCC1>[CH:18]([N:12]1[CH2:11][C:10]2[CH:13]=[CH:14][CH:15]=[CH:16][C:9]=2[S:8][C:7]2[CH:17]=[C:3]([O:2][CH3:1])[CH:4]=[CH:5][C:6]1=2)=[O:20]

Participants

4

Reactant 2

HCID 75269Acetic-formic anhydrideHCID 14126426HCID 14126426, compound

Product 1

HCID 14126428HCID 14126428, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Conditions

Temperature
2.5 °C

Procedure

To a solution of 10,11-dihydro-7-methoxydibenzo[b,f][1,4]thiazepin (6.5 g,26.6 mmoles) in tetrahydrofuran (100 ml) was added 5 ml of formic acetic anhydride. The mixture was stirred at from 0 to 5° C. for 15 minutes. The mixture was then concentrated in vacuo. The residue was taken up in ether and a solid crystallized out. The solid was filtered, washed with ether and air-dried to give the title compound, m.p. 98°-100°.

Workup

  1. concentrationThe mixture was then concentrated in vacuo
  2. customa solid crystallized out
  3. filtrationThe solid was filtered
  4. washwashed with ether
  5. customair-dried

Sources & evidence

ORD record
ord-d6096b83be8f41ccb2009ba112f184f4
Source dataset
uspto-grants-1988_03
Patent number
US04728735

Reaction notes

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