Hydrochloric Acid → HCID 178478600、化合物

HRID 462825ノート

反応式

HRID 462825 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[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]3)[CH:13]=2)=[N:5]S(=O)[N:3]=1.[ClH:26]>CO.C(O)C>[ClH:26].[ClH:26].[ClH:26].[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])[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 5486883L 643441

生成物 1

HCID 178478600HCID 178478600、化合物収率 82.6%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 887Methanol溶媒

実験手順

A suspension of 3-amino-4-[3-(3-piperidinomethylphenoxy)propylamino]-1,2,5-thiadiazole 1-oxide (17.1 g; 47.0 mmoles) [prepared according to published U.K. patent application No. 2,067,987] in 450 mL of methanol was treated with 38 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 colorless crystals. These were suspended in 200 mL of absolute ethanol, filtered and dried under vacuum to give 16.6 g (82.6%) of the title compound, m.p. 205°-222° C. (dec.). Recrystallization from 50% methanolethyl acetate gave an analytical sample, m.p. 206°-216° C. (dec.).

後処理

  1. customprepared
  2. customConcentration of the solution followed by azeotropic removal of water with absolute ethanol
  3. customgave colorless crystals
  4. filtrationfiltered
  5. customdried under vacuum

出典と根拠

ORDレコード
ord-23d7b205aba94656a52994ba0f87afa1
出典データセット
uspto-grants-1985_05
特許番号
US04517366

反応ノート

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