Water → 5-chloro-N-(2,2,3,3,4,4,4-heptafluorobutyl)-N-methyl-pentanesulfonamide

HRID 742952ノート

反応式

HRID 742952 の反応式
Cl.[F:2][C:3]([F:14])([C:7]([F:13])([F:12])[C:8]([F:11])([F:10])[F:9])[CH2:4][NH:5][CH3:6].C(N(CC)CC)C.[Cl:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][S:28](Cl)(=[O:30])=[O:29].O>C(Cl)Cl>[Cl:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][S:28]([N:5]([CH2:4][C:3]([F:14])([F:2])[C:7]([F:12])([F:13])[C:8]([F:9])([F:10])[F:11])[CH3:6])(=[O:30])=[O:29]

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 12589202HCID 12589202、化合物HCID 19711030N-(2,2,3,3,4,4,4-heptafluorobutyl)-N-methylamine hydrochloride

生成物 1

HCID 197110325-chloro-N-(2,2,3,3,4,4,4-heptafluorobutyl)-N-methyl-pentanesulfonamide収率 101.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

500 mg of N-(2,2,3,3,4,4,4-heptafluorobutyl)-N-methylamine hydrochloride (obtained according to European Patent No. 384,842 Example 75) and then, at 0° to 5° C., 0.55 ml of triethylamine were added to a solution of 200 mg of 5-chloropentane sulfonyl chloride in 5 ml of methylene chloride, and the mixture was stirred at ambient temperature for 2 hours. Water was added and extraction was carried out with methylene chloride. The extracts were washed with water, then with a saturated aqueous solution of sodium chloride, dried and evaporated to dryness under reduced pressure to obtain 378 mg of the expected product.

後処理

  1. extractionextraction
  2. washThe extracts were washed with water
  3. dry with materialwith a saturated aqueous solution of sodium chloride, dried
  4. customevaporated to dryness under reduced pressure

出典と根拠

ORDレコード
ord-cc4a513edc624cf086f8940b14efdc17
出典データセット
uspto-grants-1996_09
特許番号
US05556845

反応ノート

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