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Hydrochloric Acid → HCID 13881294、化合物

HRID 231579
ノート
印刷プレビュー

反応式

HRID 231579 の反応式
Cl[S:2]([C:5]1[CH:14]=[CH:13][CH:12]=[C:11]([N+:15]([O-:17])=[O:16])[C:6]=1[C:7]([O:9][CH3:10])=[O:8])(=[O:4])=[O:3].[NH2:18][CH2:19][CH2:20][CH2:21][OH:22].Cl>C1COCC1>[OH:22][CH2:21][CH2:20][CH2:19][NH:18][S:2]([C:5]1[CH:14]=[CH:13][CH:12]=[C:11]([N+:15]([O-:17])=[O:16])[C:6]=1[C:7]([O:9][CH3:10])=[O:8])(=[O:4])=[O:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 90863-Amino-1-propanolHCID 13670189Methyl 2-(chlorosulfonyl)-6-nitrobenzoate

生成物 1

HCID 13881294HCID 13881294、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of methyl 2-chlorosulfonyl-6-nitrobenzoate (2.80g, 10 mmol) in 100 ml of THF was cooled to ice temperature and stirred in an ice-bath while a solution of 3-amino-1-propanol (99%) (1.67g, 22 mmol) was added dropwise over a period of 45 minutes. Stirring in the ice-bath was continued for 30 minutes. The reaction miture than was acidified by addition of 3.0 ml of 1.2N HCl. The THF was evaporated under reduced pressure and the residue taken up in 100 ml of ethyl acetate. After extracting this solution with 4×20 ml of saturated NaCl solution, the ethyl acetate was evaporated and the residue recrystallized from a mixture of ethyl acetate and hexane to give 2.70g (84.9%) of light yellow crystalline product, m.p., 87-88.5°.

後処理

  1. additionwas added dropwise over a period of 45 minutes
  2. customThe THF was evaporated under reduced pressure
  3. extractionAfter extracting this solution with 4×20 ml of saturated NaCl solution
  4. customthe ethyl acetate was evaporated
  5. customthe residue recrystallized from a mixture of ethyl acetate and hexane
  6. customto give 2.70g (84.9%) of light yellow crystalline product, m.p., 87-88.5°

出典と根拠

ORDレコード
ord-395cd1fe17174bf9804b6379f43a918a
出典データセット
uspto-grants-1989_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04847294

反応ノート

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