Ammonia → HCID 86651606, 화합물

HRID 1372911노트

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HRID 1372911 반응식
[C:1](Cl)(Cl)=[O:2].[C:5]([O:9][C:10](=[O:32])[NH:11][C:12]([CH3:31])([CH3:30])[CH2:13][CH2:14][NH:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[C:22]([OH:29])([CH2:26][CH2:27][CH3:28])[CH2:23][CH2:24][CH3:25])([CH3:8])([CH3:7])[CH3:6].C(N(CC)CC)C.N>CCOC(C)=O.C1COCC1>[CH3:31][C:12]([NH:11][C:10](=[O:32])[O:9][C:5]([CH3:6])([CH3:7])[CH3:8])([CH3:30])[CH2:13][CH2:14][N:15]1[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[C:22]([CH2:23][CH2:24][CH3:25])([CH2:26][CH2:27][CH3:28])[O:29][C:1]1=[O:2]

참가 물질

7

반응물 4

HCID 222AmmoniaHCID 6371PhosgeneHCID 8471TriethylamineHCID 86600980Tert-butyl {3-[2-(1-hydroxy-1-propylbutyl)phenylamino]-1,1-dimethylpropyl}carbamate

생성물 1

HCID 86651606HCID 86651606, 화합물

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

8.85 mL (16.81 mmol) phosgene solution (20 wt. % in toluene) are slowly added dropwise at 0° C. to a solution of 6.00 g (15.28 mmol) tert-butyl{3-[2-(1-hydroxy-1-propyl-butyl)-phenylamino]-1,1-dimethyl-propyl}-carbamate and 5.32 mL (38.21 mmol) triethylamine in abs. THF (80 mL). The mixture is stirred for 2 h at RT, diluted with EtOAc, combined with ice and made basic with sat. aqueous ammonia solution. The aqueous phase is exhaustively extracted with EtOAc and the combined org. phases are washed with saturated aqueous NaCl, dried with sodium sulphate and evaporated down i. vac. After column chromatography (silica gel, cyclohexane/EtOAc 6:1) the product is obtained as a yellow oil. Yield: 4.57 g (71%).

후처리

  1. extractionThe aqueous phase is exhaustively extracted with EtOAc
  2. washphases are washed with saturated aqueous NaCl
  3. dry with materialdried with sodium sulphate
  4. customevaporated down i
  5. customAfter column chromatography (silica gel, cyclohexane/EtOAc 6:1) the product is obtained as a yellow oil

출처 및 근거

ORD 기록
ord-a86e204d4d5d474d9831e881edceb45e
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07160882B2

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