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Thiophosgene → HCID 54130839, 화합물

HRID 1858082
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HRID 1858082 반응식
C(=O)([O-])[O-].[Ca+2].[C:6](Cl)(Cl)=[S:7].[C:10]([O:14][C:15]([N:17]1[CH2:22][CH2:21][CH2:20][CH2:19][CH:18]1[CH2:23][CH2:24][O:25][C:26]1[C:35]2[C:30](=[CH:31][C:32]([Cl:37])=[C:33]([NH2:36])[CH:34]=2)[NH:29][C:28](=[O:38])[C:27]=1[C:39]1[CH:44]=[C:43]([CH3:45])[CH:42]=[C:41]([CH3:46])[CH:40]=1)=[O:16])([CH3:13])([CH3:12])[CH3:11]>O.C(Cl)(Cl)Cl>[C:10]([O:14][C:15]([N:17]1[CH2:22][CH2:21][CH2:20][CH2:19][CH:18]1[CH2:23][CH2:24][O:25][C:26]1[C:35]2[C:30](=[CH:31][C:32]([Cl:37])=[C:33]([N:36]=[C:6]=[S:7])[CH:34]=2)[NH:29][C:28](=[O:38])[C:27]=1[C:39]1[CH:40]=[C:41]([CH3:46])[CH:42]=[C:43]([CH3:45])[CH:44]=1)=[O:16])([CH3:11])([CH3:13])[CH3:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10040ThiophosgeneHCID 10112Calcium CarbonateHCID 54025520HCID 54025520, 화합물

생성물 1

HCID 54130839HCID 54130839, 화합물

시약·촉매·용매 1

HCID 22418719Chloroform water용매

실험 절차

To a stirred suspension of calcium carbonate (320 mg) and thiophosgene (120 mg) in 10 mL water:chloroform (1:1) at 0° C. was added 2-{2-[6-amino-7-chloro-3-(3,5-dimethylphenyl)-2-oxo-1,2-dihydro-quinolin-4-yloxy]-ethyl}-piperidine-1-carboxylic acid tert-butyl ester (450 mg, prepared essentially as described in Example 1) and the mixture stirred at low temperature. After 2 hours the reaction was quenched by the addition of 10% hydrochloric acid and stirring continued until the gas evolution ceased. The mixture was then extracted with chloroform, the combined organics dried over magnesium sulfate and concentrated in vacuo to provide the crude title compound (480 mg).

후처리

  1. customprepared essentially
  2. customAfter 2 hours the reaction was quenched by the addition of 10% hydrochloric acid
  3. stirringstirring
  4. extractionThe mixture was then extracted with chloroform
  5. dry with materialthe combined organics dried over magnesium sulfate
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-0a09545b6299460d84f53035fa6b2bb0
출처 데이터셋
uspto-grants-2000_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06150352

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