Diethyl Ether → 5-(4-[2-(2,2,2-Trifluoroethyl)guanidino]pyrimid-2-yloxy)valeramidine hydrochloride

HRID 2291326ノート

反応式

HRID 2291326 の反応式
[F:1][C:2]([F:24])([F:23])[CH2:3][N:4]=[C:5]([NH2:22])[NH:6][C:7]1[CH:12]=[CH:11][N:10]=[C:9]([O:13][CH2:14][CH2:15][CH2:16][CH2:17][C:18](=[NH:21])OC)[N:8]=1.[Cl-:25].[NH4+:26].CCOCC>CO>[ClH:25].[F:1][C:2]([F:24])([F:23])[CH2:3][N:4]=[C:5]([NH2:22])[NH:6][C:7]1[CH:12]=[CH:11][N:10]=[C:9]([O:13][CH2:14][CH2:15][CH2:16][CH2:17][C:18]([NH2:26])=[NH:21])[N:8]=1

参加物

5

反応物 3

HCID 3283Diethyl EtherHCID 25517Ammonium ChlorideHCID 21279807Methyl 5-(4-[2-(2,2,2-trifluoroethyl)guanidino]pyrimid-2-yloxy)valerimidate

生成物 1

HCID 212797305-(4-[2-(2,2,2-Trifluoroethyl)guanidino]pyrimid-2-yloxy)valeramidine hydrochloride収率 95.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Methyl 5-(4-[2-(2,2,2-trifluoroethyl)guanidino]pyrimid-2-yloxy)valerimidate (1.5 g.) in MeOH (15 ml.) was treated with ammonium chloride (0.25 g.) and the solution stirred at room temperature for 2 hours. Ether was added until the solution became cloudy. Continued stirring caused precipitation of a solid which was filtered to give 5-(4-[2-(2,2,2-trifluoroethyl)guanidino]pyrimid-2-yloxy)valeramidine hydrochloride, (1.52 g.), m.p. 156°-158°.

後処理

  1. stirringContinued stirring
  2. customprecipitation of a solid which
  3. filtrationwas filtered

出典と根拠

ORDレコード
ord-d516a44a5aca40deb1aba7d8773b3ef1
出典データセット
uspto-grants-1989_01
特許番号
US04795755

反応ノート

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