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Triethylamine → 2-[3-(5-Chloro-2-methoxyphenyl)-thioureido]acetamide

HRID 1449599
ノート
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反応式

HRID 1449599 の反応式
Cl.[NH2:2][CH2:3][C:4]([NH2:6])=[O:5].C(N(CC)CC)C.[Cl:14][C:15]1[CH:16]=[CH:17][C:18]([O:24][CH3:25])=[C:19]([N:21]=[C:22]=[S:23])[CH:20]=1>C(Cl)(Cl)Cl>[Cl:14][C:15]1[CH:16]=[CH:17][C:18]([O:24][CH3:25])=[C:19]([NH:21][C:22](=[S:23])[NH:2][CH2:3][C:4]([NH2:6])=[O:5])[CH:20]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 7371654-Chloro-2-isothiocyanato-1-methoxy-benzeneHCID 2723639Glycinamide hydrochloride

生成物 1

HCID 537435902-[3-(5-Chloro-2-methoxyphenyl)-thioureido]acetamide収率 94%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

A mixture of glycinamide hydrochloride (5.5 g), triethyl amine (5.05 g), 5-chloro-2-methoxyphenyl-isothiocyanate (9.95 g), and chloroform (500 mL) were heated at reflux for 3 hours. The mixture was then cooled to ambient temperature and washed with water (300 mL). The organic phase was separated. Precipitate formed upon standing. The solid was collected by filtration, washed with water, then with diethyl ether and air dried to give 2-[3-(5-chloro-2-methoxyphenyl)-thioureido]acetamide (12.8 g), m.p. 166°-169° C. (dec.). This compound was used without further purification for the preparation of the title compound.

後処理

  1. temperaturewere heated
  2. temperatureat reflux for 3 hours
  3. washwashed with water (300 mL)
  4. customThe organic phase was separated
  5. customPrecipitate formed
  6. filtrationThe solid was collected by filtration
  7. washwashed with water
  8. dry with materialwith diethyl ether and air dried

出典と根拠

ORDレコード
ord-14a3996b22604e6490053441ab350307
出典データセット
uspto-grants-1997_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05599829

反応ノート

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