Benzene → 2,2-Dichloro-1-(1-oxa-5-azaspiro[5.5]undecan-5-yl)ethan-1-one

HRID 127485ノート

反応式

HRID 127485 の反応式
[C:1]1(=[O:7])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[NH2:8][CH2:9][CH2:10][CH2:11]O.C1C=CC=CC=1.[Cl:19][CH:20]([Cl:24])[C:21](Cl)=[O:22]>O>[Cl:19][CH:20]([Cl:24])[C:21]([N:8]1[C:1]2([CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]2)[O:7][CH2:11][CH2:10][CH2:9]1)=[O:22]

参加物

6

反応物 4

HCID 241BenzeneHCID 6593Dichloroacetyl chlorideHCID 7967CyclohexanoneHCID 90863-Amino-1-propanol

生成物 1

HCID 132772052,2-Dichloro-1-(1-oxa-5-azaspiro[5.5]undecan-5-yl)ethan-1-one

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

From a boiling mixture of 17.6 g. (0.18 moles) of cyclohexanone and 11.2 g. (0.15 moles) of 3-aminopropanol in 50 ml. of benzene the water formed is continuously distilled off. Boiling is continued until 2.7 ml. of water are separated. The reaction mixture is then cooled and 16 ml. (0.165 moles) of a 40% aqueous sodium hydroxide solution are added followed by a subsequent dropwise addition of 22.1 g. (0.15 moles) of dichloroacetyl chloride, with external salt/ice cooling.

後処理

  1. additionFrom a boiling mixture of 17.6 g
  2. distillationis continuously distilled off
  3. customof water are separated
  4. temperatureThe reaction mixture is then cooled
  5. addition(0.165 moles) of a 40% aqueous sodium hydroxide solution are added
  6. additionfollowed by a subsequent dropwise addition of 22.1 g

出典と根拠

ORDレコード
ord-d40a2305369442aa974c6de9b8e13141
出典データセット
uspto-grants-1981_03
特許番号
US04256481

反応ノート

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