Formaldehyde → HCID 49761011, 화합물

HRID 907325노트

반응식

HRID 907325 반응식
[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

참가 물질

5

반응물 3

HCID 712FormaldehydeHCID 6344DichloromethaneHCID 18348438HCID 18348438, 화합물

생성물 1

HCID 49761011HCID 49761011, 화합물

시약·촉매·용매 1

HCID 3007855Zincchloride촉매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-4211c398d5a84595bd5eea2f647d830a
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08012979B2

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