Triethylamine → tert-Butyl 3-cyanomorpholine-4-carboxylate

HRID 1351346

반응식

HRID 1351346 반응식
[NH2:1][C:2]([CH:4]1[CH2:9][O:8][CH2:7][CH2:6][N:5]1[C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])=O.C(N(CC)CC)C.FC(F)(F)C(OC(=O)C(F)(F)F)=O>C(Cl)Cl>[C:2]([CH:4]1[CH2:9][O:8][CH2:7][CH2:6][N:5]1[C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])#[N:1]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 9845Trifluoroacetic anhydrideHCID 21098189tert-Butyl 3-carbamoylmorpholine-4-carboxylate

생성물 1

HCID 21098190tert-Butyl 3-cyanomorpholine-4-carboxylate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of the product of Step 2 (1 eq.) and triethylamine (2.1 eq.) in CH2Cl2 (0.1 M) was cooled to 0° C. and-trifluoroacetic anhydride (1.1 eq.) added dropwise under nitrogen. Stirring was continued 3.5 hours more at room temperature and volatiles removed in vacuo. Residues taken in EtOAc were washed with water, brine and dried over Na2SO4. Evaporation gave the title compound as a brown solid.

후처리

  1. customvolatiles removed in vacuo
  2. washwere washed with water, brine
  3. dry with materialdried over Na2SO4
  4. customEvaporation

출처 및 근거

ORD 기록
ord-f3c939e449c645d68dd58527541c32ae
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07217713B2

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