Hydrochloric Acid → HCID 57152477, 화합물

HRID 1066572

반응식

HRID 1066572 반응식
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]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 554404Methyl chloromethanethioateHCID 86756995HCID 86756995, 화합물

생성물 1

HCID 57152477HCID 57152477, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-907faad2b0ff44d189f6e780718697d6
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06242600B1

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