Triethylamine → N-[1-(3-Chloro-[1,2,4]thiadiazol-5-yl)-piperidin-4-yl]-N-cyclopropyl-4-oxazol-5-yl-benzamide

HRID 68835노트

반응식

HRID 68835 반응식
Cl.[CH:2]1([N:5]([CH:19]2[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]2)[C:6](=[O:18])[C:7]2[CH:12]=[CH:11][C:10]([C:13]3[O:17][CH:16]=[N:15][CH:14]=3)=[CH:9][CH:8]=2)[CH2:4][CH2:3]1.[Cl:25][C:26]1[N:30]=[C:29](Cl)[S:28][N:27]=1.C(N(CC)CC)C>ClCCl>[Cl:25][C:26]1[N:30]=[C:29]([N:22]2[CH2:23][CH2:24][CH:19]([N:5]([CH:2]3[CH2:4][CH2:3]3)[C:6](=[O:18])[C:7]3[CH:8]=[CH:9][C:10]([C:13]4[O:17][CH:16]=[N:15][CH:14]=4)=[CH:11][CH:12]=3)[CH2:20][CH2:21]2)[S:28][N:27]=1

참가 물질

5

반응물 3

HCID 8471Triethylamine2회HCID 2725055Dichloro-1,2,4-thiadiazoleHCID 68289930N-cyclopropyl-4-oxazol-5-yl-N-piperidin-4-yl-benzamide hydrochloride

생성물 1

HCID 68290214N-[1-(3-Chloro-[1,2,4]thiadiazol-5-yl)-piperidin-4-yl]-N-cyclopropyl-4-oxazol-5-yl-benzamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of N-cyclopropyl-4-oxazol-5-yl-N-piperidin-4-yl-benzamide hydrogen chloride salt (696 mg), 3,5-dichloro-1,2,4-thiadiazole (372 mg), and triethylamine (0.42 mL) in dichloromethane (30 mL) is stirred overnight at room temperature. More triethylamine (0.40 mL) is added and the mixture is stirred until the conversion is complete (1 h). The solvent is partly evaporated and the residue is triturated with water. The precipitate is filtered off, washed with dichloromethane and dried to yield the title compound. LC (method 5): tR=2.08 min; Mass spectrum (ESI+): m/z=430/432 (Cl) [m+H]+.

후처리

  1. stirringthe mixture is stirred until the conversion
  2. custom(1 h)
  3. customThe solvent is partly evaporated
  4. customthe residue is triturated with water
  5. filtrationThe precipitate is filtered off
  6. washwashed with dichloromethane
  7. customdried

출처 및 근거

ORD 기록
ord-167d80cfc81f48c79b865e35021a37d7
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822471B2

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