1-Chloro-4-(chloromethyl)benzene → 2-Amino-7-(p-chloro-benzyl)-6,7,8,9-tetrahydro-5H-pyrazino[2,3-d]azepine

HRID 647484노트

반응식

HRID 647484 반응식
Br.Br.[NH2:3][C:4]1[CH:5]=[N:6][C:7]2[CH2:13][CH2:12][NH:11][CH2:10][CH2:9][C:8]=2[N:14]=1.C(N(C(C)C)C(C)C)C.[Cl:24][C:25]1[CH:32]=[CH:31][C:28]([CH2:29]Cl)=[CH:27][CH:26]=1>C(#N)C>[NH2:3][C:4]1[CH:5]=[N:6][C:7]2[CH2:13][CH2:12][N:11]([CH2:29][C:28]3[CH:31]=[CH:32][C:25]([Cl:24])=[CH:26][CH:27]=3)[CH2:10][CH2:9][C:8]=2[N:14]=1

참가 물질

5

반응물 3

HCID 77231-Chloro-4-(chloromethyl)benzeneHCID 81531DiisopropylethylamineHCID 204363772-amino-6,7,8,9-tetrahydro-5H-pyrazino[2,3-d]azepine dihydrobromide

생성물 1

HCID 130370462-Amino-7-(p-chloro-benzyl)-6,7,8,9-tetrahydro-5H-pyrazino[2,3-d]azepine

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

3.0 gm (9.2 mmols) of 2-amino-6,7,8,9-tetrahydro-5H-pyrazino[2,3-d]azepine dihydrobromide were suspended in 100 ml of acetonitrile, 7.5 ml of N-ethyl-diisopropylamine were added to the suspension, and the mixture was admixed dropwise with 1.5 gm (9.3 mmols) of p-chloro-benzyl-chloride. The reaction mixture was stirred for 48 hours and then evaporated, the residue was acidified with dilute hydrochloric acid, and the mixture was extracted with methylene chloride. The aqueous phase was made alkaline and then exhaustively extracted with methylene chloride, the extracts were evaporated, and the residue was column-chromatographically purified on silicagel with ethyl acetate as the mobile phase.

후처리

  1. customevaporated
  2. extractionthe mixture was extracted with methylene chloride
  3. extractionexhaustively extracted with methylene chloride
  4. customthe extracts were evaporated
  5. custompurified on silicagel with ethyl acetate as the mobile phase

출처 및 근거

ORD 기록
ord-68ecc466d85e45f78be21d9484e3581c
출처 데이터셋
uspto-grants-1983_10
특허 번호
US04409220

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