Isopropylamine → N-(1-Methylethyl)-4-(phenylsulfonyl)-1-butanamine hydrochloride

HRID 4205

반응식

HRID 4205 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][CH2:5][S:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)(=[O:8])=[O:7].[CH:15]([NH2:18])([CH3:17])[CH3:16]>C(Cl)(Cl)Cl.CO>[ClH:1].[CH3:16][CH:15]([NH:18][CH2:2][CH2:3][CH2:4][CH2:5][S:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)(=[O:8])=[O:7])[CH3:17]

참가 물질

5

반응물 2

HCID 6363IsopropylamineHCID 12457347((4-Chlorobutyl)sulfonyl)benzene

생성물 1

HCID 13655073N-(1-Methylethyl)-4-(phenylsulfonyl)-1-butanamine hydrochloride수율 30%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6212Chloroform용매

실험 절차

A solution of 105.95 g (0.456 mole) [(4-chlorobutyl)sulfonyl]benzene was heated overnight at 75° C. on an autoclave in 200 ml of isopropylamine. The reaction mixture was stripped to dryness. The residue obtained was dissolved in chloroform and the chloroform layer was extracted with water. The chloroform layer was dried, filtered, and solvent removed to give a dark brown oil. The oil was dissolved in methanol and converted to the hydrochloride salt. This salt was recrystallized from methanol-diethyl ether and dried in vacuo overnight at 80° C. This gave white crystalline product, m.p. 155°-157.5° C. in 30% yield.

후처리

  1. customThe residue obtained
  2. extractionthe chloroform layer was extracted with water
  3. dry with materialThe chloroform layer was dried
  4. filtrationfiltered
  5. customsolvent removed
  6. customto give a dark brown oil
  7. customThis salt was recrystallized from methanol-diethyl ether
  8. customdried in vacuo overnight at 80° C

출처 및 근거

ORD 기록
ord-95c3f93212c34abcafd8589c1a2860f7
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04724235

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