Nitrogen → Methyl-[3-(2,2,2-trifluoro-acetylamino)-propyl]-carbamic acid isopropyl ester

HRID 870672ノート

反応式

HRID 870672 の反応式
N#N.[F:3][C:4]([F:14])([F:13])[C:5]([NH:7][CH2:8][CH2:9][CH2:10][NH:11][CH3:12])=[O:6].CN1CCOCC1.Cl[C:23]([O:25][CH:26]([CH3:28])[CH3:27])=[O:24]>C(OCC)(=O)C.C1(C)C=CC=CC=1>[CH:26]([O:25][C:23](=[O:24])[N:11]([CH3:12])[CH2:10][CH2:9][CH2:8][NH:7][C:5](=[O:6])[C:4]([F:13])([F:14])[F:3])([CH3:28])[CH3:27]

参加物

7

反応物 4

HCID 947NitrogenHCID 7917Isopropyl chloroformateHCID 79724-MethylmorpholineHCID 585874312,2,2-trifluoro-N-(3-(methylamino)propyl)acetamide

生成物 1

HCID 86696374Methyl-[3-(2,2,2-trifluoro-acetylamino)-propyl]-carbamic acid isopropyl ester

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
0 °C

実験手順

To a rapidly stirred, 0° C., N2 blanketed, solution of 2,2,2-trifluoro-N-(3-methylamino-propyl)-acetamide (6.0 g, 32.4 mmol) and N-methylmorpholine [109-02-4] (7.1 mL, 64.6 mmol) in ethyl acetate (65 mL) was steadily added a 1.0M solution of isopropyl chloroformate in toluene (32.4 mL) over the course of 10 minutes. The reaction was allowed to stir and warm to ambient temperature over night at which time it was washed with brine, dried (MgSO4) and evaporated to provide 9.0 g of clear yellow oil. LRMS (ESI) m/z 271.1 [(M+H)]+, calc'd for C10H17F3N2O3: 270.25.

後処理

  1. stirringto stir
  2. temperaturewarm to ambient temperature over night at which time it
  3. washwas washed with brine
  4. dry with materialdried (MgSO4)
  5. customevaporated

出典と根拠

ORDレコード
ord-95e31ef2858845efa2a5994c6e65a2a5
出典データセット
uspto-grants-2015_03
特許番号
US08969565B2

反応ノート

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