Hydrochloric Acid → (3-Chloro-3-methyl-2-nitrosobutoxy)benzene

HRID 263219ノート

反応式

HRID 263219 の反応式
[ClH:1].[O:2]([CH2:9][CH:10]=[C:11]([CH3:13])[CH3:12])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[N:14]([O:16]CCCCC)=O>C(O)(=O)C>[Cl:1][C:11]([CH3:13])([CH:10]([N:14]=[O:16])[CH2:9][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1)[CH3:12]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 10026Pentyl nitriteHCID 564931Benzene, ((3-methyl-2-butenyl)oxy)-

生成物 1

HCID 21316467(3-Chloro-3-methyl-2-nitrosobutoxy)benzene収率 22%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

Concentrated hydrochloric acid (8.1 ml) was added dropwise over 10 minutes to a mixture of 1-(p-methoxy)phenoxy-3-methylbut-2-ene (VI; R=CH2OC6H4.OCH3, R1 =R2 =CH3) (16.05 g) and amyl nitrite (12.1 ml) in glacial acetic acid (16.2 ml) at -5° to 0° (ice-salt bath). After a further 1 hour at -5° to 0°, the mixture was filtered. The solid so obtained was washed with acetone and recrystallised from acetone to give the nitrosochloride (V) (4.87 g, yield 22%) as pale yellow crystals, m.p. 123° (decomp.).

後処理

  1. filtrationthe mixture was filtered
  2. customThe solid so obtained
  3. washwas washed with acetone
  4. customrecrystallised from acetone

出典と根拠

ORDレコード
ord-2bfe99ea7ee74202848a2b6dafdf129a
出典データセット
uspto-grants-1979_05
特許番号
US04156725

反応ノート

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