Water → HCID 12939990, compound
Reaction equation
[CH3:1][N:2]([CH3:6])[C:3](Cl)=[O:4].[Cl:7][C:8]1[CH:9]=[CH:10][C:11]2[S:15]C(NC)=[N:13][C:12]=2[CH:18]=1.[H-].[Na+].O.[CH3:22][N:23](C)[CH:24]=O>>[Cl:7][C:8]1[CH:9]=[CH:10][C:11]2[S:15][C:1]([N:2]([CH3:6])[C:3](=[O:4])[N:23]([CH3:24])[CH3:22])=[N:13][C:12]=2[CH:18]=1Participants
6
Procedure
N,N-dimethylcarbamoylchloride (1.1g) and 5-chloro-2-methylaminobenzothiazole (2g) were dissolved in dimethylformamide (25ml) and the mixture was stirred while adding slowly sodiumhydride (0.44g, 55% oily) in a stream of nitrogen for an hour and maintaining the temperature below -5°C. After stirring 3 additional hours at the room temperature, the mixture was poured into water (100ml) and the precipitate was filtrated, washed and dried.
Workup
- temperaturemaintaining the temperature below -5°C
- stirringAfter stirring 3 additional hours at the room temperature
- filtrationthe precipitate was filtrated
- washwashed
- customdried
Sources & evidence
- ORD record
- ord-93aeb2eedfd243db89beedaef9d512b2
- Source dataset
- uspto-grants-1976_07
- Patent number
- US03967950
Reaction notes
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