6-Amidino-1-carbamoylmethyl-2-naphthyl 4-nitrobenzoate.hydrochloride → 6-Amidino-1-carbamoylmethyl-2-naphthyl 4-aminobenzoate.dihydrochloride

HRID 1419226ノート

反応式

HRID 1419226 の反応式
[ClH:1].[N+:2]([C:5]1[CH:30]=[CH:29][C:8]([C:9]([O:11][C:12]2[CH:21]=[CH:20][C:19]3[C:14](=[CH:15][CH:16]=[C:17]([C:22](=[NH:24])[NH2:23])[CH:18]=3)[C:13]=2[CH2:25][C:26](=[O:28])[NH2:27])=[O:10])=[CH:7][CH:6]=1)([O-])=O>[C].[Pd].CN(C=O)C>[ClH:1].[ClH:1].[NH2:2][C:5]1[CH:6]=[CH:7][C:8]([C:9]([O:11][C:12]2[CH:21]=[CH:20][C:19]3[C:14](=[CH:15][CH:16]=[C:17]([C:22](=[NH:23])[NH2:24])[CH:18]=3)[C:13]=2[CH2:25][C:26](=[O:28])[NH2:27])=[O:10])=[CH:29][CH:30]=1

参加物

4

反応物 1

HCID 701312286-Amidino-1-carbamoylmethyl-2-naphthyl 4-nitrobenzoate.hydrochloride

生成物 1

HCID 701325966-Amidino-1-carbamoylmethyl-2-naphthyl 4-aminobenzoate.dihydrochloride収率 188.1%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 6228Dimethylformamide溶媒

実験手順

To 600 mg of 6-amidino-1-carbamoylmethyl-2-naphthyl 4-nitrobenzoate.hydrochloride were added 10 ml of anhydrous DMF and 100 mg of 10% palladium carbon, and catalytic reduction was effected at room temperature for 24 hours. Then, insoluble matter was filtered off and the filtrate was concentrated under reduced pressure. To the residue was added 15 ml of methanol, and, furthermore, 350 μl of concentrated hydrochloric acid was added with stirring under cooling with ice. Then, the resulting solution was added dropwise to 200 ml of acetone, followed by stirring for 1 hour under cooling with ice. Then, the precipitate was collected by filtration to obtain 572.7 mg of the desired product.

後処理

  1. filtrationThen, insoluble matter was filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. additionTo the residue was added 15 ml of methanol
  4. additionfurthermore, 350 μl of concentrated hydrochloric acid was added
  5. temperatureunder cooling with ice
  6. additionThen, the resulting solution was added dropwise to 200 ml of acetone
  7. stirringby stirring for 1 hour
  8. temperatureunder cooling with ice
  9. filtrationThen, the precipitate was collected by filtration

出典と根拠

ORDレコード
ord-5d8cdbd579214dfe9cd1f14c441aa46d
出典データセット
uspto-grants-1999_03
特許番号
US05885990

反応ノート

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