Hydroxyamine hydrochloride → 1-Benzyl 4-chloro-2,3,6,7-tetrahydro-5-oximinomethylene-1H-azepine hydrochloride

HRID 1648924노트

반응식

HRID 1648924 반응식
Cl.[CH2:2]([N:9]1[CH2:15][CH2:14][C:13]([CH:16]=O)=[C:12]([Cl:18])[CH2:11][CH2:10]1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.Cl.[NH2:20][OH:21]>C(O)C>[ClH:18].[CH2:2]([N:9]1[CH2:15][CH2:14][C:13](=[C:16]=[N:20][OH:21])[CH:12]([Cl:18])[CH2:11][CH2:10]1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1

참가 물질

4

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 189435411-benzyl-5-chloro-2,3,6,7-tetrahydro-1H-azepine-4-carbaldehyde hydrochloride

생성물 1

HCID 867391081-Benzyl 4-chloro-2,3,6,7-tetrahydro-5-oximinomethylene-1H-azepine hydrochloride

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

45 gm (0.16 mol) of 1-benzyl-4-chloro-5-formyl-2,3,6,7-tetrahydro-1H-azepine hydrochloride were suspended in 450 ml of ethyl alcohol, and at 30° C. 12.2 gm (0.175 mol) of hydroxylamine hydrochloride were added in batches while stirring. After some hours, a crystalline precipitate separated out of the gradually clearing solution. The reaction mixture was stirred for 2 hours more and then allowed to stand overnight. The crystalline precipitate was suction-filtered off and dried. After evaporation of the mother liquor, another 10 gm were obtained.

후처리

  1. customat 30° C
  2. waitAfter some hours
  3. customa crystalline precipitate separated out of the gradually clearing solution
  4. stirringThe reaction mixture was stirred for 2 hours more
  5. filtrationThe crystalline precipitate was suction-filtered off
  6. customdried
  7. customAfter evaporation of the mother liquor
  8. customanother 10 gm were obtained

출처 및 근거

ORD 기록
ord-5fb27cbf32a543e3a9e3ceb9efe7c1c7
출처 데이터셋
uspto-grants-1983_11
특허 번호
US04414225

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