Formic Acid → HCID 10176502, compound

HRID 1079321Notes

Reaction equation

HRID 1079321 reaction equation
[S:1]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[CH2:5][NH:4][CH2:3][CH2:2]1.[CH:12](O)=[O:13]>C1(C)C=CC=CC=1>[CH:12]([N:4]1[CH2:5][C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=2[S:1][CH2:2][CH2:3]1)=[O:13]

Participants

4

Reactant 2

HCID 284Formic AcidHCID 122691062,3,4,5-Tetrahydrobenzo[f][1,4]thiazepine

Product 1

HCID 10176502HCID 10176502, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Conditions

Temperature
90 °C

Procedure

A mixture of 2,3,4,5-tetrahydro-1,4-benzothiazepine (4.56 g), formic acid (20 ml) and toluene (60 ml) was heated under reflux at 90° C. for four hours and then at 120° C. for a further three hours. The solvent was removed from the mixture by evaporation at reduced pressure. Purification of the residue by flash chromatography using dichloromethane as eluent gave 4-formyl-2,3,4,5-tetrahydro-1,4-benzothiazepine, which was recrystallised from hexane. Yield 3.73 g (m.p. 84°-87° C.).

Workup

  1. temperaturewas heated
  2. customThe solvent was removed from the mixture by evaporation at reduced pressure
  3. customPurification of the residue by flash chromatography

Sources & evidence

ORD record
ord-9dd6271a847447f4a1ebfc07c4491aac
Source dataset
uspto-grants-1996_12
Patent number
US05580866

Reaction notes

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