Hydrochloric Acid → 4-(Benzyloxy)butanimidamide--hydrogen chloride (1/1)

HRID 544566노트

반응식

HRID 544566 반응식
[CH2:1]([O:8][CH2:9][CH2:10][CH2:11][C:12]#[N:13])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CCO.[ClH:17].[NH4+:18].[Cl-]>C(Cl)Cl.CO>[ClH:17].[CH2:1]([O:8][CH2:9][CH2:10][CH2:11][C:12]([NH2:18])=[NH:13])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 25517Ammonium ChlorideHCID 20458213Butanenitrile, 4-(phenylmethoxy)-

생성물 1

HCID 204582074-(Benzyloxy)butanimidamide--hydrogen chloride (1/1)

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

A solution of 4-benzyloxybutyronitrile (16.5 g.) and EtOH (8.6 g.) in CH2Cl2 (100 ml.) was saturated with HCl gas at 0° and the mixture kept at 0° for 6 days. The resulting suspension was evaporated to dryness in vacuo and the residue was slurried with dry ether. The insoluble solid was added to 40% aqueous K2CO3 (120 g.) at 0° and the oil which separated was extracted with CH2Cl2 (2×100 ml.). The CH2Cl2 layer was washed with a little water, brine and then dried to give the crude imidate (14 g.). This was stirred with NH4Cl (3.5 g.) in MeOH (100 ml.) for 24 hours and the solution was evaporated to give a crude sample (14.6 g.) of 4-benzyloxybutanamidine hydrochloride.

후처리

  1. customThe resulting suspension was evaporated to dryness in vacuo
  2. additionThe insoluble solid was added to 40% aqueous K2CO3 (120 g.) at 0°
  3. customthe oil which separated
  4. extractionwas extracted with CH2Cl2 (2×100 ml.)
  5. washThe CH2Cl2 layer was washed with a little water, brine
  6. customdried
  7. customto give the crude imidate (14 g.)
  8. customthe solution was evaporated

출처 및 근거

ORD 기록
ord-425769538c9c41858351b939d69b0122
출처 데이터셋
uspto-grants-1984_05
특허 번호
US04451463

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