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

HRID 68835ノート

反応式

HRID 68835 の反応式
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

参加物

5

反応物 3

HCID 8471Triethylamine2 回HCID 2725055Dichloro-1,2,4-thiadiazoleHCID 68289930N-cyclopropyl-4-oxazol-5-yl-N-piperidin-4-yl-benzamide hydrochloride

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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]+.

後処理

  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

出典と根拠

ORDレコード
ord-167d80cfc81f48c79b865e35021a37d7
出典データセット
uspto-grants-2014_09
特許番号
US08822471B2

反応ノート

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