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

HRID 1351346

反応式

HRID 1351346 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-f3c939e449c645d68dd58527541c32ae
出典データセット
uspto-grants-2007_05
特許番号
US07217713B2

関連ノート

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