Trichloroacetonitrile → (4-Bromophenyl)(thien-3-yl)methyl 2,2,2-trichloroethammidoate

HRID 1180388ノート

反応式

HRID 1180388 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:10]2[CH:14]=[CH:13][S:12][CH:11]=2)[OH:9])=[CH:4][CH:3]=1.[H-].[Na+].[Cl:17][C:18]([Cl:22])([Cl:21])[C:19]#[N:20]>C(OCC)C>[Cl:17][C:18]([Cl:22])([Cl:21])[C:19](=[NH:20])[O:9][CH:8]([C:5]1[CH:4]=[CH:3][C:2]([Br:1])=[CH:7][CH:6]=1)[C:10]1[CH:14]=[CH:13][S:12][CH:11]=1

参加物

5

反応物 3

HCID 11011TrichloroacetonitrileHCID 24758Sodium hydrideHCID 49962536(4-Bromophenyl)(thiophen-3-yl)methanol

生成物 1

HCID 69473113(4-Bromophenyl)(thien-3-yl)methyl 2,2,2-trichloroethammidoate

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

To a solution of (4-bromophenyl)(thien-3-yl)methanol from step 1 (632 mg, 2.36 mmol) in diethyl ether (2.5 mL) at 0° C. was added sodium hydride (6 mg, 0.24 mmol). Then trichloroacetonitrile was added dropwise (237 μL, 2.36 mmol) over 15 minutes and the reaction was allowed to warm to room temperature for 3 hours. The reaction was then filtered over celite and concentrated under reduced pressure. The resulting crude compound was used as such in the next step.

後処理

  1. filtrationThe reaction was then filtered over celite and
  2. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-75e5a14f24f343bbb1f14ea62e29a683
出典データセット
uspto-grants-2007_10
特許番号
US07279478B2

反応ノート

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