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

HRID 127485노트

반응식

HRID 127485 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d40a2305369442aa974c6de9b8e13141
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04256481

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