1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 18426157、化合物

HRID 2187802ノート

反応式

HRID 2187802 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([CH:12]=[CH:13][CH:14]=1)[C:5]([NH:7][CH2:8][C:9]([OH:11])=O)=[O:6].CCN=C=NCCCN(C)C.O.ON1C2C=CC=CC=2N=N1.Cl.Cl.[Cl:39][C:40]1[CH:53]=[CH:52][C:43]([CH2:44][N:45]2[CH2:50][CH2:49][CH2:48][CH:47]([NH2:51])[CH2:46]2)=[CH:42][CH:41]=1>C(Cl)(Cl)Cl.CCN(CC)CC>[Cl:39][C:40]1[CH:41]=[CH:42][C:43]([CH2:44][N:45]2[CH2:50][CH2:49][CH2:48][CH:47]([NH:51][C:9](=[O:11])[CH2:8][NH:7][C:5](=[O:6])[C:4]3[CH:12]=[CH:13][CH:14]=[C:2]([CH3:1])[CH:3]=3)[CH2:46]2)=[CH:52][CH:53]=1

参加物

7

反応物 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 992233-Methylhippuric AcidHCID 27960291-Hydroxybenzotriazole hydrateHCID 18426178HCID 18426178、化合物

生成物 1

HCID 18426157HCID 18426157、化合物

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 8471Triethylamine溶媒

反応条件

温度
25 °C

実験手順

N-(3-Methylbenzoyl)glycine (10.6 mg, 0.055 mmol), EDCI (10.5 mg) and 1-hydroxybenzotriazole hydrate (7.4 mg) were added to a solution of 1-(4-chlorobenzyl)-3-aminopiperidine dihydrochloride (14.9 mg, 0.050 mmol) and Et3N (15.2 mg) in CHCl3 (2.5 mL). The reaction mixture was stirred at 25° C. for 16 h, washed with 2 N aqueous NaOH (2 mL×2) and brine (1 mL). After filtration through PTFE membrane filter, the solvent was removed under reduced pressure to afford 1-(4-chlorobenzyl)-3-[{N-(3-methylbenzoyl)glycyl}amino]piperidine (compound No. 355) as a pale yellow oil (17.4 mg, 87%): The purity was determined by RPLC/MS (97%); ESI/MS m/e 400.0 (M++H, C22H26ClN3O2).

後処理

  1. washwashed with 2 N aqueous NaOH (2 mL×2) and brine (1 mL)
  2. filtrationAfter filtration through PTFE membrane
  3. filtrationfilter
  4. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-e3c4b097f6284e11a887f6daf63113c4
出典データセット
uspto-grants-2002_06
特許番号
US06410566B1

反応ノート

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