Hydrochloric Acid → HCID 178478599、化合物

HRID 370824ノート

反応式

HRID 370824 の反応式
[NH2:1][C:2]1[C:6]([NH:7][CH2:8][CH2:9][CH2:10][O:11][C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([CH2:18][N:19]3[CH2:23][CH2:22][CH2:21][CH2:20]3)[CH:13]=2)=[N:5]S(=O)[N:3]=1.[ClH:25]>CO>[ClH:25].[ClH:25].[ClH:25].[N:19]1([CH2:18][C:14]2[CH:13]=[C:12]([CH:17]=[CH:16][CH:15]=2)[O:11][CH2:10][CH2:9][CH2:8][NH:7][C:6](=[NH:5])[C:2](=[NH:1])[NH2:3])[CH2:23][CH2:22][CH2:21][CH2:20]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 159612053-Amino-4-[3-(3-pyrrolidinomethylphenoxy)propylamino]-1,2,5-thiadiazole 1-oxide

生成物 1

HCID 178478599HCID 178478599、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A suspension of 3-amino-4-[3-(3-pyrrolidinomethylphenoxy)propylamino]-1,2,5-thiadiazole 1-oxide (13.4 g; 38.3 mmoles) [prepared according to published U.K. patent application No. 2,067,987] in 350 mL of methanol was treated with 25.5 mL of concentrated HCl. The resultant solution was stirred for 3 hours at ambient temperature. Concentration of the solution followed by azeotropic removal of water with absolute ethanol gave the product. The crystalline residue was triturated with 150 mL of absolute ethanol, filtered and dried to give 10.8 g of the title compound, m.p. 195°-203° C. (dec.).

後処理

  1. customprepared
  2. customConcentration of the solution followed by azeotropic removal of water with absolute ethanol
  3. customgave the product
  4. customThe crystalline residue was triturated with 150 mL of absolute ethanol
  5. filtrationfiltered
  6. customdried

出典と根拠

ORDレコード
ord-493521e49f6f40dcadbaafe8ea618bd1
出典データセット
uspto-grants-1985_07
特許番号
US04528378

反応ノート

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