Sodium Bicarbonate → HCID 178512547、化合物

HRID 2292129ノート

反応式

HRID 2292129 の反応式
[O:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[O:7][CH2:8][CH2:9][S:10][C:11]1[CH:16]=[CH:15][C:14]([OH:17])=[CH:13][CH:12]=1.[NH:18]([C:22]1[CH:30]=[CH:29][C:25]([C:26](Cl)=[O:27])=[CH:24][CH:23]=1)[C:19]([NH2:21])=[NH:20].[C:31]([O-:34])([OH:33])=[O:32].[Na+]>N1C=CC=CC=1>[C:31](=[O:32])([OH:34])[OH:33].[NH:18]([C:22]1[CH:30]=[CH:29][C:25]([C:26]([O:17][C:14]2[CH:13]=[CH:12][C:11]([S:10][CH2:9][CH2:8][O:7][CH:2]3[CH2:3][CH2:4][CH2:5][CH2:6][O:1]3)=[CH:16][CH:15]=2)=[O:27])=[CH:24][CH:23]=1)[C:19]([NH2:21])=[NH:20]

参加物

5

反応物 3

HCID 516892Sodium BicarbonateHCID 140519404-Hydroxyphenyl 2-(tetrahydropyran-2-yloxy)ethyl sulfide2 回HCID 178512519HCID 178512519、化合物

生成物 1

HCID 178512547HCID 178512547、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

96.08 g of 4-hydroxyphenyl 2-(tetrahydropyran-2-yloxy)ethyl sulfide synthesized by the above process (2) was dissolved in 800 ml of pyridine. 4-Guanidinobenzoyl chloride was added to the solution under cooling with ice and the mixture was stirred at room temperature for 24 h or longer. A saturated aqueous sodium hydrocarbonate solution was added thereto under cooling with ice and the precipitate thus obtained was recovered by filtration, washed with water, then acetone and finally ethyl acetate and dried to obtain 104 g of 4-(2-tetrahydropyran-2-yloxyethylthio)phenyl 4-guanidinobenzoate carbonate.

後処理

  1. temperatureunder cooling with ice
  2. temperatureunder cooling with ice
  3. customthe precipitate thus obtained
  4. filtrationwas recovered by filtration
  5. washwashed with water
  6. dry with materialacetone and finally ethyl acetate and dried

出典と根拠

ORDレコード
ord-420ad075b4ae453d9cdaca7d04116add
出典データセット
uspto-grants-1989_01
特許番号
US04801603

反応ノート

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