Hydrochloric Acid → HCID 68511847, 화합물

HRID 1404946노트

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HRID 1404946 반응식
[N:1]1([C:11](=[O:23])[CH2:12][S:13][C:14]2[S:15][C:16]3[CH:21]=[CH:20][N:19]=[CH:18][C:17]=3[N:22]=2)[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][CH2:2]1.[ClH:24]>CCOCC.CCO>[ClH:24].[N:1]1([C:11](=[O:23])[CH2:12][S:13][C:14]2[S:15][C:16]3[CH:21]=[CH:20][N:19]=[CH:18][C:17]=3[N:22]=2)[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][CH2:2]1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 59467884HCID 59467884, 화합물

생성물 1

HCID 68511847HCID 68511847, 화합물수율 77%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 3283Diethyl Ether용매

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온도
0 °C

실험 절차

Compound 69 (162 mg, 4.7 mmol) was dissolved in 10 mL of Et2O and 2.5 mL of EtOH, stirred for 10 min, then 0.57 mL of 1M HCl (in Et2O) was added slowly. The precipitation started upon addition of the acid. The reaction mixture was stirred for 1 h at RT, 40 min at 0° C., filtered. The precipitate washed with Et2O and dried under high vacuum over P4O10 overnight, then at 45° C. for 4 h to yield compound 70 (150 mg, 77%): MS: m/z+ 342.1 (M+H)+; Anal. Calcd (found) for C17H16ClN3OS2: C, 54.03 (53.78); H, 4.27 (4.33); N, 11.12 (10.95); Cl, 9.38 (9.15); S, 16.97 (16.68).

후처리

  1. customThe precipitation
  2. additionstarted upon addition of the acid
  3. filtrationfiltered
  4. washThe precipitate washed with Et2O
  5. dry with materialdried under high vacuum over P4O10 overnight

출처 및 근거

ORD 기록
ord-de419a28b3be46359dd805965f4c6d14
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08916550B2

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