Hydrochloric Acid → HCID 178478600, 화합물

HRID 745865노트

반응식

HRID 745865 반응식
[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

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 5486883L 643441

생성물 1

HCID 178478600HCID 178478600, 화합물수율 82.6%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 887Methanol용매

실험 절차

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 United Kingdom 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.).

후처리

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

출처 및 근거

ORD 기록
ord-f7c2ff35e1124d93a80cae0feb9f6375
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04600779

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