Water → HCID 59043085, 화합물

HRID 2120972노트

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HRID 2120972 반응식
[C:1]([O:5][C:6](=[O:23])[C@@H:7]([NH:13][S:14]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)(=[O:16])=[O:15])[CH2:8][CH2:9][C:10](O)=[O:11])([CH3:4])([CH3:3])[CH3:2].ClC(OCC)=O.[C:30]1([CH2:36][N:37]2[CH2:42][CH2:41][C:40]3([CH2:47][CH2:46][NH:45][CH2:44][CH2:43]3)[CH2:39][CH2:38]2)[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1.O>C1COCC1.C(N(CC)CC)C>[C:17]1([S:14]([NH:13][C@@H:7]([CH2:8][CH2:9][C:10](=[O:11])[N:45]2[CH2:46][CH2:47][C:40]3([CH2:39][CH2:38][N:37]([CH2:36][C:30]4[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=4)[CH2:42][CH2:41]3)[CH2:43][CH2:44]2)[C:6]([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:23])(=[O:15])=[O:16])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 10928Ethyl chloroformateHCID 4195333-Benzyl-3,9-diazaspiro[5.5]undecaneHCID 59043077HCID 59043077, 화합물

생성물 1

HCID 59043085HCID 59043085, 화합물

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회HCID 8471Triethylamine용매

실험 절차

A solution of 6.82 g (19.86 mmol) of the intermediate from Step B in 20 ml dry THF containing 2.8 ml triethylamine was cooled to −10° C. 2.15 g (19.8 mmol) ethyl chloroformate were added dropwise, and the mixture was stirred for ten minutes, while a precipitate was formed spontaneously. A solution of 4.85 g (19.86 mmol) of the intermediate from Example 20, Step D in a mixture of 24 ml dry THF and 5.3 ml triethylamine was added quickly in small portions. It was warmed to room temperature, stirred over night, poured into water, and extracted three times with ethyl acetate. The combined organic layers were washed with water, dried over sodium sulfate, and concentrated under reduced pressure, and the title compound was obtained by chromatography on silica gel with dichloromethane/ethanol 93:7.

후처리

  1. customwas formed spontaneously
  2. additionwas added quickly in small portions
  3. stirringstirred over night
  4. extractionextracted three times with ethyl acetate
  5. washThe combined organic layers were washed with water
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-8e4ae1f0003245d88becd90f6b973bb2
출처 데이터셋
uspto-grants-2004_02
특허 번호
US06693109B2

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