Triethylamine → HCID 3828237、化合物

HRID 2363998ノート

反応式

HRID 2363998 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 3828237HCID 3828237、化合物収率 95.1%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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:

後処理

  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)

出典と根拠

ORDレコード
ord-271cecbefb5a4605ab851763c0f9ba20
出典データセット
uspto-grants-2014_04
特許番号
US08691828B2

反応ノート

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