Formaldehyde → HCID 49761011、化合物

HRID 907325ノート

反応式

HRID 907325 の反応式
[F:1][C:2]([F:18])([F:17])[C:3]([N:5]1[CH2:10][CH2:9][CH:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH2:7][CH2:6]1)=[O:4].C=O.[Cl:21][CH2:22]Cl>[Cl-].[Cl-].[Zn+2]>[Cl:21][CH2:22][C:14]1[CH:15]=[CH:16][C:11]([CH:8]2[CH2:9][CH2:10][N:5]([C:3](=[O:4])[C:2]([F:1])([F:17])[F:18])[CH2:6][CH2:7]2)=[CH:12][CH:13]=1

参加物

5

反応物 3

HCID 712FormaldehydeHCID 6344DichloromethaneHCID 18348438HCID 18348438、化合物

生成物 1

HCID 49761011HCID 49761011、化合物

試薬・触媒・溶媒 1

HCID 3007855Zincchloride触媒

実験手順

A suspension of the product of step i) (18 g), paraformaldehyde (14 g) and zinc dichloride (14 g) in dichloromethane (700 mL) was stirred at room temperature. Hydrogen chloride gas was bubbled through the reaction for 30 minutes. The reaction was stirred at room temperature under a blanket of nitrogen for a further 18 hours. Water (150 mL) was added and the phases separated. The organic phase was dried using magnesium sulfate and concentrated in vacuo to give a green oil which was purified (SiO2 eluting with 30% i-hexane in dichloromethane) to give the sub-title compound (12 g).

後処理

  1. customHydrogen chloride gas was bubbled through the reaction for 30 minutes
  2. stirringThe reaction was stirred at room temperature under a blanket of nitrogen for a further 18 hours
  3. additionWater (150 mL) was added
  4. customthe phases separated
  5. customThe organic phase was dried
  6. concentrationconcentrated in vacuo
  7. customto give a green oil which
  8. customwas purified (SiO2 eluting with 30% i-hexane in dichloromethane)

出典と根拠

ORDレコード
ord-4211c398d5a84595bd5eea2f647d830a
出典データセット
uspto-grants-2011_09
特許番号
US08012979B2

反応ノート

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