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Ethyl chloroformate → Benzamide, 4-(acetylamino)-5-chloro-N-[(2-ethyloctahydrocyclopenta[c]pyrrol-1-yl)methyl]-2-methoxy-

HRID 1833407
ノート
印刷プレビュー

反応式

HRID 1833407 の反応式
[CH3:1][O:2][C:3]1[CH:11]=[C:10]([NH:12][C:13](=[O:15])[CH3:14])[C:9]([Cl:16])=[CH:8][C:4]=1[C:5]([OH:7])=O.ClC(OCC)=O.[CH2:23]([N:25]1[CH2:32][CH:31]2[CH:27]([CH2:28][CH2:29][CH2:30]2)[CH:26]1[CH2:33][NH2:34])[CH3:24]>O1CCCC1.C(N(CC)CC)C>[CH2:23]([N:25]1[CH2:32][CH:31]2[CH:27]([CH2:28][CH2:29][CH2:30]2)[CH:26]1[CH2:33][NH:34][C:5](=[O:7])[C:4]1[CH:8]=[C:9]([Cl:16])[C:10]([NH:12][C:13](=[O:15])[CH3:14])=[CH:11][C:3]=1[O:2][CH3:1])[CH3:24]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 10928Ethyl chloroformateHCID 109884964-Acetamido-5-chloro-2-methoxybenzoic acidHCID 85848305HCID 85848305、化合物

生成物 1

HCID 86733791Benzamide, 4-(acetylamino)-5-chloro-N-[(2-ethyloctahydrocyclopenta[c]pyrrol-1-yl)methyl]-2-methoxy-

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒2 回
HCID 8471
Triethylamine
溶媒

反応条件

温度
0 °C

実験手順

To a suspension of 6 parts of 2-methoxy-4-acetylamino-5-chloro benzoic acid in 50 parts of anhydrous tetrahydrofuran, were added 2.5 parts of triethylamine. The solution thus obtained was poured portionwise in a mixture of 2.7 parts of ethyl chloroformate in 80 parts of tetrahydrofuran maintained at 0° C. After stirring for 10 minutes, 4.1. parts of N-ethyl-2-aminomethyl-3-azabicyclo (3,3,0) octane were added. After being maintained at room temperature for 10 minutes, the temperature was progressively increased and, finally, the reaction mixture was refluxed for 60 minutes. After cooling, the mixture was filtered and the filtrate was evaporated in vacuo. After recrystallization in 50 parts of ethyl acetate, there were obtained 5.5 parts of N-ethyl-2-(2-methoxy-4-acetylamino-5-chloro benzamido methyl)-3-azabicyclo (3,3,0) octane, M.P. 156°-157° C (ethyl acetate).

後処理

  1. customThe solution thus obtained
  2. temperatureAfter being maintained at room temperature for 10 minutes
  3. temperaturethe temperature was progressively increased
  4. temperaturefinally, the reaction mixture was refluxed for 60 minutes
  5. temperatureAfter cooling
  6. filtrationthe mixture was filtered
  7. customthe filtrate was evaporated in vacuo
  8. customAfter recrystallization in 50 parts of ethyl acetate

出典と根拠

ORDレコード
ord-cfafa8d9228a466abce7c71a51184e64
出典データセット
uspto-grants-1978_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04066662

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート