Ethanol → Dimaprit hydrochloride
反応式
[ClH:1].[Cl:2][CH2:3][CH2:4][CH2:5][N:6]([CH3:8])[CH3:7].[NH2:9][C:10]([NH2:12])=[S:11].C(O)C>C(OCC)(=O)C>[ClH:2].[ClH:1].[CH3:7][N:6]([CH3:8])[CH2:5][CH2:4][CH2:3][S:11][C:10](=[NH:9])[NH2:12]参加物
5
実験手順
A stirred mixture of 1-chloro-3-(dimethylamino) propane hydrochloride (305.7 g), thiourea (150 g) and ethanol (1530 ml) was heated under reflux for 24 hours then cooled to ambient temperature. Ethyl acetate was added until a faint opalescence was observed, then the mixture was stored at 4° C. for 72 hours. The resulting solid was collected by filtration, washed with ethyl acetate, and dried in vacuo at 40° C. to give S-[3-(dimethylamino)propyl]isothiourea dihydrochloride as a white solid (403 g), m.p. 155°-157° C.
後処理
- temperaturewas heated
- temperatureunder reflux for 24 hours
- filtrationThe resulting solid was collected by filtration
- washwashed with ethyl acetate
- customdried in vacuo at 40° C.
出典と根拠
- ORDレコード
- ord-d879c6ecc91548d8a9020fa25c28e991
- 出典データセット
- uspto-grants-1997_07
- 特許番号
- US05652271
反応ノート
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