Triethylamine → HCID 54040071, 화합물

HRID 233742

반응식

HRID 233742 반응식
CC([O-])(C)C.[K+].Cl.[NH2:8][C@@H:9]([CH2:14][CH2:15][CH2:16]C)[C:10]([O:12][CH3:13])=[O:11].C(N(CC)CC)C.[Br:25][C:26]1[CH:31]=[CH:30][C:29]([CH2:32]Br)=[CH:28][N:27]=1>COCCOC.CN(C=O)C>[Br:25][C:26]1[N:27]=[CH:28][C:29]([CH2:32][NH:8][C@H:9]([C:10]([O:12][CH3:13])=[O:11])[CH2:14][CH2:15][CH3:16])=[CH:30][CH:31]=1

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 64246602-Bromo-5-bromomethylpyridineHCID 14039065methyl (2S)-2-aminohexanoate hydrochlorideHCID 23665647Potassium tert-butoxide

생성물 1

HCID 54040071HCID 54040071, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매2회HCID 80711,2-Dimethoxyethane용매

반응 조건

온도
20 °C

실험 절차

1.48 g (13.2 mmol) of potassium tert-butylate are added to a solution of 2.18 g (12 mmol) of methyl (S)-2-aminohexanoate hydrochloride and 1.66 ml of triethylamine in 20 ml of DME and 15 ml of DMF under argon. After stirring at 20° C. for 1 h, a solution of 3.01 g (12 mmol) of 2-bromo-5-bromomethylpyridine in 15 ml of DMF is injected and the mixture is stirred for 16 h. Subsequently, the solvent is distilled off in vacuo and the residue is taken up in dichloromethane/water; the organic phase is then dried over sodium sulphate and, after concentrating, purified on silica gel using petroleum ether/ethyl acetate (4:1).

후처리

  1. stirringthe mixture is stirred for 16 h
  2. distillationSubsequently, the solvent is distilled off in vacuo
  3. dry with materialthe organic phase is then dried over sodium sulphate
  4. concentrationafter concentrating
  5. custompurified on silica gel

출처 및 근거

ORD 기록
ord-e392811c6725432ca09c3d03f743034d
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05594010

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