Phosgene → 4-Isocyanato-7-methoxy-4,5,6,7-tetrahydro-1-benzothiophene
Reaction equation
[CH3:1][O:2][CH:3]1[C:8]2[S:9][CH:10]=[CH:11][C:7]=2[CH:6]([NH2:12])[CH2:5][CH2:4]1.[C:13](Cl)(Cl)=[O:14]>>[CH3:1][O:2][CH:3]1[C:8]2[S:9][CH:10]=[CH:11][C:7]=2[CH:6]([N:12]=[C:13]=[O:14])[CH2:5][CH2:4]1Participants
3
Procedure
A 1 g sample of 4,5,6,7-tetrahydro-7-methoxybenzo[b]thiophen-4-amine is added to 18 ml of 12.5% phosgene solution (benzene) in a nitrogen atmosphere at 20° C. After stirring at room temperature for an hour, the mixture is heated to 60° C and kept at this temperature for 7 hours. The mixture is cooled to room temperature and evaporated to dryness in vacuo to afford the crude 4,5,6,7-tetrahydro-7-methoxybenzo[b]thien-4-ylisocyanate.
Workup
- temperaturethe mixture is heated to 60° C
- temperatureThe mixture is cooled to room temperature
- customevaporated to dryness in vacuo
Sources & evidence
- ORD record
- ord-89bcf8129df24c1093551b7c4b58f227
- Source dataset
- uspto-grants-1976_12
- Patent number
- US03998959
Reaction notes
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