Hydrochloric Acid → HCID 178478600, 화합물

HRID 370806노트

반응식

HRID 370806 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 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% methanol-ethyl acetate gave an analytical sample, m.p. 206°-216° C. (dec.).

후처리

  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

출처 및 근거

ORD 기록
ord-b2a81617ab70445aa7259311d9b4b9e6
출처 데이터셋
uspto-grants-1985_07
특허 번호
US04528375

반응 노트

불러오는 중…