4-Formylbenzoic acid → Tert-butyl 4-(4-formylbenzoyl)piperazine-1-carboxylate

HRID 13554

반응식

HRID 13554 반응식
[C:1]([C:4]1[CH:11]=[CH:10][C:7]([CH:8]=[O:9])=[CH:6][CH:5]=1)([OH:3])=O.[C:12]([O:16][C:17]([N:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1)=[O:18])([CH3:15])([CH3:14])[CH3:13].CCN=C=NCCCN(C)C.Cl.C1C=CC2N(O)N=NC=2C=1>C(Cl)Cl.CN(C)C1C=CN=CC=1>[C:12]([O:16][C:17]([N:19]1[CH2:24][CH2:23][N:22]([C:1](=[O:3])[C:4]2[CH:11]=[CH:10][C:7]([CH:8]=[O:9])=[CH:6][CH:5]=2)[CH2:21][CH2:20]1)=[O:18])([CH3:15])([CH3:13])[CH3:14]

참가 물질

7

반응물 4

HCID 120884-Formylbenzoic acidHCID 757711-HydroxybenzotriazoleHCID 143452tert-Butyl piperazine-1-carboxylateHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

생성물 1

HCID 59218188Tert-butyl 4-(4-formylbenzoyl)piperazine-1-carboxylate

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

A suspension of 4-carboxybenzaldehyde (3.10 g) in CH2Cl2 was treated sequentially with piperazine-1-carboxylic acid tert-butyl ester (3.6 g), EDCl (3.86 g), HOBt (2.68 g), and 4-dimethylaminopyridine (˜0.020 g). After 18 h, the mixture was extracted with 1 N NaOH and then with 1 N HCl. The organic layer was dried (Na2SO4) and concentrated to yield the title compound.

후처리

  1. extractionthe mixture was extracted with 1 N NaOH
  2. dry with materialThe organic layer was dried (Na2SO4)
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-9f2266dfe35b4b34a5f82d1e7a0771b8
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728129B2

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