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Water → HCID 22000405, 화합물

HRID 1976137
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HRID 1976137 반응식
Cl.[NH2:2][CH2:3][CH:4]1[CH2:9][CH2:8][CH:7]([NH:10][C:11](=[O:20])[O:12][CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH2:6][CH2:5]1.C(N(C(C)C)CC)(C)C.[C:30]([N:38]=[C:39]=[S:40])(=[O:37])[C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1.O>C1COCC1>[CH2:13]([O:12][C:11](=[O:20])[NH:10][CH:7]1[CH2:8][CH2:9][CH:4]([CH2:3][NH:2][C:39]([NH:38][C:30](=[O:37])[C:31]2[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=2)=[S:40])[CH2:5][CH2:6]1)[C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1
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참가 물질

6

반응물 4

HCID 962WaterHCID 68284Benzoyl isothiocyanateHCID 81531DiisopropylethylamineHCID 22990186trans-4-(Cbz-amino)cyclohexanemethanamine hydrochloride

생성물 1

HCID 22000405HCID 22000405, 화합물수율 101.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran
용매

실험 절차

A solution of benzyl N-[4-(aminomethyl)cyclohexyl]carbamate HCl (3.46 g, 11.58 mmol) and diisopropylethylamine (6.0 ml) in anhydrous THF (90 ml) was stirred at room temperature for 20 minutes. To this solution was added benzoylisothiocyanate (2.00 g, 12.3 mmol). The solution was stirred at room temperature for 14 hours, poured into water (200 ml) and then extracted with Et2O (2×150 ml). The organic layer was dried over MgSO4, filtered and evaporated to yield a solid. The solid was triturated with hexane and filtered to yield 99% (5.023 g) of the desired product.

후처리

  1. extractionextracted with Et2O (2×150 ml)
  2. dry with materialThe organic layer was dried over MgSO4
  3. filtrationfiltered
  4. customevaporated
  5. customto yield a solid
  6. customThe solid was triturated with hexane
  7. filtrationfiltered

출처 및 근거

ORD 기록
ord-9c79faec768441959242f5ba37fe2590
출처 데이터셋
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06225330B1

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