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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Carbamate → HCID 22669293, 화합물

HRID 1018256
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HRID 1018256 반응식
[C:1](=[O:4])([O-])[NH2:2].[CH:5]([C:7]1[CH:17]=[CH:16][C:10]([O:11][CH2:12][C:13]([OH:15])=O)=[CH:9][CH:8]=1)=[O:6].[CH3:18][CH2:19][N:20](C(C)C)C(C)C.CN(C(O[N:35]1[N:43]=[N:42][C:37]2[CH:38]=[CH:39][CH:40]=[CH:41][C:36]1=2)=[N+](C)C)C.[B-](F)(F)(F)F>Cl.O1CCOCC1.C(Cl)Cl.CCOC(C)=O>[N:42]([C:37]1[CH:36]=[CH:41][C:40]([C:1]([NH:2][CH2:18][CH2:19][NH:20][C:13](=[O:15])[CH2:12][O:11][C:10]2[CH:9]=[CH:8][C:7]([CH:5]=[O:6])=[CH:17][CH:16]=2)=[O:4])=[CH:39][CH:38]=1)=[N+:43]=[N-:35]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 276CarbamateHCID 81531DiisopropylethylamineHCID 89177Acetic acid, 2-(4-formylphenoxy)-HCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate

생성물 1

HCID 22669293HCID 22669293, 화합물

시약·촉매·용매 3

HCID 6344Dichloromethane
용매
HCID 8857Ethyl Acetate용매
HCID 204431481,4-Dioxane hydrochloride용매

실험 절차

The crude carbamate (0.257 g, 0.84 mmol) was deprotected by stirring in 4N HCl-dioxane (15 mL) for 2 h at room temperature. Volatiles were removed under reduced pressure to give a pinkish solid. 4-Formylphenoxyacetic acid (0.200 g, 1.1 mmol) was dissolved in DCM (3 mL) and DIEA (0.5 mL) was added followed by TBTU (0.350 g, 1,1 mmol) and the amine salt from above (0.240 g, 1 mmol). The mixture was stirred 4 h at room temperature, dissolved in EtOAc and washed sequentially with 5% aqueous K2CO3, KHSO4, water and brine. The extract was dried (MgSO4) and concentrated under reduced pressure to give an off-white solid (0.162 g).

후처리

  1. customVolatiles were removed under reduced pressure
  2. customto give a pinkish solid
  3. washwashed sequentially with 5% aqueous K2CO3, KHSO4, water and brine
  4. dry with materialThe extract was dried (MgSO4)
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-2d741b07c2ea4387b161e80f61bd703b
출처 데이터셋
uspto-grants-2002_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06479508B1

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