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Hydrochloric Acid → HCID 178427282、化合物

HRID 462827
ノート
印刷プレビュー

反応式

HRID 462827 の反応式
[NH2:1][C:2]1[C:6]([NH:7][CH2:8][CH2:9][S:10][CH2:11][C:12]2[S:13][C:14]([CH2:18][N:19]([CH3:21])[CH3:20])=[C:15]([CH3:17])[CH:16]=2)=[N:5]S(=O)[N:3]=1.[ClH:23]>CO>[ClH:23].[ClH:23].[ClH:23].[CH3:21][N:19]([CH2:18][C:14]1[S:13][C:12]([CH2:11][S:10][CH2:9][CH2:8][NH:7][C:6](=[NH:5])[C:2](=[NH:1])[NH2:3])=[CH:16][C:15]=1[CH3:17])[CH3:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 23312524HCID 23312524、化合物

生成物 1

HCID 178427282HCID 178427282、化合物収率 80%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A stirred solution of 3-amino-4-{2-[(5-dimethylaminomethyl-4-methyl-2-thienyl)methylthio]ethylamino}-1,2,5-thiadiazole 1-oxide (17.9 g, 50.0 mmoles) [prepared according to the general procedure described in published U.K. patent application No. 2,067,987] in 500 mL of methanol was treated with 33.3 mL of concentrated HCl. After stirring for 3 hours, the reaction mixture was concentrated and excess water was removed by azeotropic concentration with absolute ethanol to give an almost colorless crystalline residue. The residue was triturated with 200 mL of absolute ethanol at 0° C., filtered and dried to give 16.9 g (80%) of the title compound, m.p. 206°-220° C. (dec.). Recrystallization from 50% methanolethyl acetate gave a product having m.p. 210°-221° C. (dec.).

後処理

  1. concentrationthe reaction mixture was concentrated
  2. customexcess water was removed by azeotropic concentration with absolute ethanol
  3. customto give an almost colorless crystalline residue
  4. customThe residue was triturated with 200 mL of absolute ethanol at 0° C.
  5. filtrationfiltered
  6. customdried

出典と根拠

ORDレコード
ord-3166f1d5ef554a2db1df97ba4d2e5751
出典データセット
uspto-grants-1985_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04517366

反応ノート

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