Triethylamine → HCID 27866014, 화합물

HRID 384848노트

반응식

HRID 384848 반응식
Cl.[CH2:2](N=C=NCCCN(C)C)C.Cl.[CH2:14]([O:21][C:22]1[CH:29]=[CH:28][C:25]([CH2:26][NH2:27])=[CH:24][C:23]=1[O:30][CH3:31])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.[C:32]([O:36][C:37]([N:39]1[CH2:43][CH2:42][C@H:41]([C:44]([OH:46])=O)[CH2:40]1)=[O:38])([CH3:35])([CH3:34])[CH3:33].C(N(CC)CC)C>C(Cl)Cl>[CH2:14]([O:21][C:22]1[CH:29]=[CH:28][C:25]([CH2:26][NH:27][C:44]([C@H:41]2[CH2:2][CH2:42][CH2:43][N:39]([C:37]([O:36][C:32]([CH3:33])([CH3:34])[CH3:35])=[O:38])[CH2:40]2)=[O:46])=[CH:24][C:23]=1[O:30][CH3:31])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 1512492(3S)-1-[(tert-butoxy)carbonyl]pyrrolidine-3-carboxylic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 162477591-[4-(Benzyloxy)-3-methoxyphenyl]methanamine--hydrogen chloride (1/1)

생성물 1

HCID 27866014HCID 27866014, 화합물수율 69.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1-Ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (1.12 g) was added to a mixture of 4-benzyloxy-3-methoxybenzylamine hydrochloride (1.26 g), (S)-1-(t-butoxycarbonyl)pyrrolidine-3-carboxylic acid (0.97 g), triethylamine (0.82 ml) and methylene chloride (20 ml). After stirring the reaction mixture at room temperature for 20 hours, the mixture was washed with saturated ammonium chloride aqueous solution and then saturated brine, the organic layer was dried over sodium sulfate and the solvent was evaporated under reduced pressure. The residue was purified by silica gel chromatography (elution solvent: hexane/ethyl acetate=100/0 to 0/100 gradient) to obtain 1.42 g of t-butyl (S)-3-(4-benzyloxy-3-methoxybenzylcarbamoyl)-piperidine-1-carboxylate.

후처리

  1. washthe mixture was washed with saturated ammonium chloride aqueous solution
  2. dry with materialsaturated brine, the organic layer was dried over sodium sulfate
  3. customthe solvent was evaporated under reduced pressure
  4. customThe residue was purified by silica gel chromatography (elution solvent: hexane/ethyl acetate=100/0 to 0/100 gradient)

출처 및 근거

ORD 기록
ord-d3a4482c5e4647ba810198af6a42f1b1
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08367835B2

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