Acetic Acid → HCID 178443033, 화합물

HRID 839900노트

반응식

HRID 839900 반응식
Cl.Cl.C(S[C:6](=[NH:47])[C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([CH2:13][N:14]([CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH3:46])[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])[CH:8]=1)C.[CH:48]1([NH2:53])[CH2:52][CH2:51][CH2:50][CH2:49]1.C(O)(=O)C>C(Cl)(Cl)Cl>[CH2:31]([N:14]([CH2:13][C:9]1[CH:8]=[C:7]([CH:12]=[CH:11][CH:10]=1)[C:6]([NH:53][CH:48]1[CH2:52][CH2:51][CH2:50][CH2:49]1)=[NH:47])[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])[CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH3:46]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 2906CyclopentylamineHCID 12565115Ethyl-m-[N,N-di(n-hexadecyl)aminomethyl]-thiobenzimidate Dihydrochloride

생성물 1

HCID 178443033HCID 178443033, 화합물수율 77%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

Ethyl-m-[N,N-di(n-hexadecyl)aminomethyl]-thiobenzimidate dihydrochloride (1.074 g., 1.5 mmoles) was added to a solution of cyclopentylamine (255 mg., 3.0 mmoles, glacial acetic acid (0.3 ml., 5.3 mmoles) and chloroform (10 ml.). The mixture was held for 72 hours at room temperature. It was then diluted to 300 ml. with chloroform, washed with saturated aqueous sodium bicarbonate solution (3 × 50 ml.), washed with saturated aqueous sodium chloride solution (3 × 50 ml.), dried (Na2 SO4) and filtered. The filtrate was acidified with a 10% solution of anhydrous hydrogen chloride in dioxane (5ml.) and then evaporated in vacuo to an oil. The oil was crystallized from warm 1,2-dimethoxyethane [850 mg., 77% yield, Rf .30 (4:1, benzene:ethanol on silicic acid), m.p.--forms a gel at 78° C.].

후처리

  1. additionIt was then diluted to 300 ml
  2. washwith chloroform, washed with saturated aqueous sodium bicarbonate solution (3 × 50 ml.)
  3. washwashed with saturated aqueous sodium chloride solution (3 × 50 ml.)
  4. customdried (Na2 SO4)
  5. filtrationfiltered
  6. customevaporated in vacuo to an oil
  7. customThe oil was crystallized
  8. temperaturefrom warm 1,2-dimethoxyethane [850 mg
  9. customat 78° C.

출처 및 근거

ORD 기록
ord-1da25338006e42c7982145c8edd74e69
출처 데이터셋
uspto-grants-1978_06
특허 번호
US04097525

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