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

HRID 4205

反応式

HRID 4205 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-95c3f93212c34abcafd8589c1a2860f7
出典データセット
uspto-grants-1988_02
特許番号
US04724235

関連ノート

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