Hydrochloric Acid → HCID 57152477、化合物

HRID 1066572ノート

反応式

HRID 1066572 の反応式
FC(F)(F)[C:3]([OH:5])=O.[NH2:8][C@@H:9]([CH2:28][C:29](=[O:42])[N:30]1[CH2:35][CH2:34][N:33]([C:36]2[CH:41]=[CH:40][N:39]=[CH:38][CH:37]=2)[CH2:32][CH2:31]1)[C:10]([N:12]1[CH2:17][CH2:16][N:15]([CH2:18][C:19]([OH:21])=[O:20])[C:14](=[O:22])[C@@:13]1([CH:25]=[C:26]=[O:27])OC)=[O:11].[C:43](=O)([O-])O.[Na+].Cl[C:49](OC)=[S:50].Cl>O1CCOCC1.O>[CH3:43][C:49]([NH:8][C@@H:9]([CH2:28][C:29](=[O:42])[N:30]1[CH2:35][CH2:34][N:33]([C:36]2[CH:37]=[CH:38][N:39]=[CH:40][CH:41]=2)[CH2:32][CH2:31]1)[C:10]([N:12]1[CH2:17][CH2:16][N:15]([CH2:18][C:19]([OH:21])=[O:20])[C:14](=[O:22])[C@H:13]1[CH2:25][C:26]([O:5][CH3:3])=[O:27])=[O:11])=[S:50]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 554404Methyl chloromethanethioateHCID 86756995(r,s)-[4-[2-Amino-4-oxo-4-[4-(pyridin-4-yl)piperazin-1-yl]butyryl]-3-methoxy-carbonylmethyl-2-oxopiperazin-1-yl]acetic acid trifluoroacetic acid salt

生成物 1

HCID 57152477HCID 57152477、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

To a mixture of (R,S)-[4-[2-amino-4-oxo-4-[4-(pyridin-4-yl)piperazin-1-yl]butyryl]-3-methoxy-carbonylmethyl-2-oxopiperazin-1-yl]acetic acid trifluoroacetic acid salt (0.25 g) produced in Working Example 21, an aqueous solution of sodium hydrogen carbonate (0.15 g), water (2.5 ml) and 1,4-dioxane (2.5 ml)was added methyl chlorothioformate (0.047 ml) and the solution was stirred for 1 hour at room temperature. To the reaction solution was added 1N hydrochloric acid and the solution was adjusted to pH 3, which was concentrated under reduced pressure. The concentrate was purified by CHP-20 column chromatography (eluent:H2O→10% acetonitrile aqueous solution). The objected fraction was concentrated and subjected to lyophilization to give the titled compound (0.18 g) as a white amorphous powdery product.

後処理

  1. customproduced in Working Example 21
  2. concentrationwas concentrated under reduced pressure
  3. customThe concentrate was purified by CHP-20 column chromatography (eluent:H2O→10% acetonitrile aqueous solution)
  4. concentrationThe objected fraction was concentrated

出典と根拠

ORDレコード
ord-907faad2b0ff44d189f6e780718697d6
出典データセット
uspto-grants-2001_06
特許番号
US06242600B1

反応ノート

読み込み中…