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Ethyl trifluoroacetate → Acetamide, N-(2-aminocyclohexyl)-2,2,2-trifluoro-, cis-

HRID 711561
ノート
印刷プレビュー

反応式

HRID 711561 の反応式
[C@@H:1]1([NH2:8])[CH2:6][CH2:5][CH2:4][CH2:3][C@@H:2]1[NH2:7].[F:9][C:10]([F:17])([F:16])[C:11](OCC)=[O:12]>CCO>[NH2:7][C@H:2]1[CH2:3][CH2:4][CH2:5][CH2:6][C@H:1]1[NH:8][C:11](=[O:12])[C:10]([F:17])([F:16])[F:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 9794Ethyl trifluoroacetateHCID 3429171,2-Diaminocyclohexane, cis-

生成物 1

HCID 11042018Acetamide, N-(2-aminocyclohexyl)-2,2,2-trifluoro-, cis-

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

cis-Cyclohexane-1,2-diamine (5.00 g, 43.9 mmol, 1.00 eq) was charged to a 250 ml, three-neck round bottom flask equipped with an overhead stirrer and a thermocouple. Ethanol (50 mL) was added and the solution was cooled to <0° C. using an ice-brine bath. A solution of ethyl trifluoroacetate (6.23 g, 1.00 eq) in EtOH (25 mL) was added via a syringe pump over a one hour period. Once the addition was complete, the cooling bath was removed and the solution was slowly warmed to RT and stirred for 3.5 hours to afford the title compound in EtOH. Half (41 mL, about 21.9 mmol) of the total solution (about 82 mL) was carried into the next step.

後処理

  1. customequipped with an overhead stirrer
  2. temperaturethe solution was cooled to <0° C.
  3. additionOnce the addition
  4. customthe cooling bath was removed

出典と根拠

ORDレコード
ord-62478a3501d04b30ba976b92bb573c84
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09181255B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート