Triethylamine → HCID 3828237, 화합물

HRID 2363998노트

반응식

HRID 2363998 반응식
[O:1]1[C:5]2([CH2:10][CH2:9][NH:8][CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1.C(N(CC)CC)C.Cl[C:19]([O:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)=[O:20]>C(OCC)(=O)C>[O:1]1[C:5]2([CH2:10][CH2:9][N:8]([C:19]([O:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)=[O:20])[CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 15891Phenyl chloroformateHCID 674351,4-Dioxa-8-azaspiro(4.5)decane

생성물 1

HCID 3828237HCID 3828237, 화합물수율 95.1%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To a stirred solution of 1,4-dioxa-8-azaspiro[4.5]decane (2.00 g, 13.9 mmol) and triethylamine (2.90 mL, 20.9 mmol) in ethyl acetate (50 mL) at 0° C. was added phenyl chloroformate (2.10 mL, 13.9 mmol). The mixture was allowed to warm to room temperature overnight. Then, the mixture was filtered to remove triethylamine hydrochloride salts. The filtrate was concentrated, and the obtained residue was chromatographed (silica gel, hexanes to 50:50 hexanes/ethyl acetate) to give the title compound (3.48 g, 95%) as a white solid:

후처리

  1. filtrationThen, the mixture was filtered
  2. customto remove triethylamine hydrochloride salts
  3. concentrationThe filtrate was concentrated
  4. customthe obtained residue was chromatographed (silica gel, hexanes to 50:50 hexanes/ethyl acetate)

출처 및 근거

ORD 기록
ord-271cecbefb5a4605ab851763c0f9ba20
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08691828B2

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