Acetic Acid → HCID 178443033、化合物

HRID 839900ノート

反応式

HRID 839900 の反応式
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]

参加物

5

反応物 3

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

生成物 1

HCID 178443033HCID 178443033、化合物収率 77%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.].

後処理

  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.

出典と根拠

ORDレコード
ord-1da25338006e42c7982145c8edd74e69
出典データセット
uspto-grants-1978_06
特許番号
US04097525

反応ノート

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