Hydrochloric Acid → HCID 21404066、化合物

HRID 972434ノート

反応式

HRID 972434 の反応式
C([O:4][C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[C:8]([S:15](Cl)(=[O:17])=[O:16])=[CH:7][CH:6]=1)(=O)C.[CH2:19]([NH:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH3:43])[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30].C(N(CC)CC)C.[OH-].[K+].Cl>CCOCC.O.C(#N)C>[CH2:32]([N:31]([CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH3:30])[S:15]([C:8]1[C:9]2[C:14](=[CH:13][CH:12]=[CH:11][CH:10]=2)[C:5]([OH:4])=[CH:6][CH:7]=1)(=[O:16])=[O:17])[CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH3:43]

参加物

9

反応物 5

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 14797Potassium HydroxideHCID 18157DidodecylamineHCID 214040784-(Chlorosulfonyl)naphthalen-1-yl acetate

生成物 1

HCID 21404066HCID 21404066、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒2 回HCID 3283Diethyl Ether溶媒HCID 6342Acetonitrile溶媒

実験手順

A mixture of 18.1 g (0.063 mole) 1-acetoxy-4-naphthalenesulfonyl chloride, 22.4 g (0.063 mole) N,N-didodecylamine, 25 ml (18.1 g, 0.18 mole) triethylamine, and 200 ml acetonitrile was stirred at room temperature for 18 hrs. The mixture was diluted with ether and poured into water. The ether layer was separated, dried, and concentrated to 16.1 g of an amber oil, which was dissolved in 100 ml ethanol. To the solution was added 1.50 g (0.027 mole) potassium hydroxide; the mixture was stirred at room temperature for 2 days, acidified with hydrochloric acid, and diluted with water. The mixture was extracted with ether, and the extract was concentrated to 30.7 g of an amber oil, which partially crystallized.

後処理

  1. customThe ether layer was separated
  2. customdried
  3. concentrationconcentrated to 16.1 g of an amber oil, which
  4. dissolutionwas dissolved in 100 ml ethanol
  5. stirringthe mixture was stirred at room temperature for 2 days
  6. extractionThe mixture was extracted with ether
  7. concentrationthe extract was concentrated to 30.7 g of an amber oil, which
  8. custompartially crystallized

出典と根拠

ORDレコード
ord-e250f05f53624c4dbb883b29fb802961
出典データセット
uspto-grants-1977_10
特許番号
US04053312

反応ノート

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