Acetic Acid → HCID 86641156、化合物

HRID 1807694ノート

反応式

HRID 1807694 の反応式
[F:1][C:2]([F:9])([F:8])[C:3]([CH3:7])([CH3:6])[C:4]#[N:5].C[O-].[Na+].[Na].C(O)(=O)C.[NH4+:18].[Cl-:19]>CO>[ClH:19].[F:1][C:2]([F:9])([F:8])[C:3]([CH3:7])([CH3:6])[C:4]([NH2:18])=[NH:5]

参加物

7

反応物 5

HCID 176Acetic AcidHCID 25517Ammonium ChlorideHCID 5360545SodiumHCID 10942334Sodium MethoxideHCID 207676543,3,3-Trifluoro-2,2-dimethyl-propionitrile

生成物 1

HCID 86641156HCID 86641156、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
70 °C

実験手順

3,3,3-Trifluoro-2,2-dimethyl-propionitrile (Stage 44.3) (12.40 mmol) was added to a solution of sodium methoxide (freshly prepared from 48.40 mmol sodium metal and 102 mL MeOH) at rt. After 4 h, acetic acid (48.40 mmol) and then NH4Cl (14.88 mmol) were slowly added and the reaction mixture was then heated to 70° C. for 40 h. After concentrating (40° C., 100 mbar) the reaction mixture, the residue was suspended in acetone, filtered and dried under vacuum to afford the title compound as a white solid. ESI-MS: [M+H]+ 155.

後処理

  1. concentrationAfter concentrating (40° C., 100 mbar) the reaction mixture
  2. filtrationfiltered
  3. customdried under vacuum

出典と根拠

ORDレコード
ord-467fea5cb28d4d7295611b618060a63f
出典データセット
uspto-grants-2013_01
特許番号
US08357707B2

反応ノート

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