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Sulfuric Acid → HCID 20326662、化合物

HRID 596171
ノート
印刷プレビュー

反応式

HRID 596171 の反応式
[C:1]([CH2:3][CH2:4][N:5]1[CH2:11][CH2:10][C:9]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[O:8][CH2:7][CH2:6]1)#[N:2].[Cl-:24].[Al+3].[Cl-].[Cl-].[H-].[Al+3].[Li+].[H-].[H-].[H-].S(=O)(=O)(O)O>C(OCC)C.O>[ClH:24].[ClH:24].[NH2:2][CH2:1][CH2:3][CH2:4][N:5]1[CH2:11][CH2:10][C:9]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)([C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)[O:8][CH2:7][CH2:6]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 1118Sulfuric AcidHCID 6451240Aluminum(III) ChlorideHCID 20326631HCID 20326631、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 20326662HCID 20326662、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 3283
Diethyl Ether
溶媒
2 回

実験手順

3.06 g of 4-(2-cyanoethyl)-7,7-diphenyl-hexahydro-1,4-oxazepine are added portionwise to the suspension prepared by combining the solution of 1.33 g of anhydrous aluminum chloride in 30 ml of diethyl ether with that of 0.38 g of lithium aluminum hydride in 30 ml of diethyl ether while stirring and cooling with an ice-bath. The mixture is allowed to warm up to room temperature, stirred for 5 1/2 hours and cooled again to 0°-5°. Thereupon 5 ml of water and 15 ml of 3N aqueous sulfuric acid are added and the organic layer extracted with 3N aqueous sulfuric acid. The aqueous layers are combined, made basic with concentrated aqueous sodium hydroxide and the mixture extracted four times with 15 ml of diethyl ether each. The extract is dried, filtered and evaporated. The residue is taken up in ethanol and the solution acidified with ethereal hydrogen chloride, to yield the 4-(3-aminopropyl)-7,7-diphenyl-hexahydro-1,4-oxazepine dihydrochloride melting at 190°-192° with decomposition.

後処理

  1. customprepared
  2. temperaturecooling with an ice-bath
  3. stirringstirred for 5 1/2 hours
  4. temperaturecooled again to 0°-5°
  5. extractionthe organic layer extracted with 3N aqueous sulfuric acid
  6. extractionthe mixture extracted four times with 15 ml of diethyl ether each
  7. customThe extract is dried
  8. filtrationfiltered
  9. customevaporated

出典と根拠

ORDレコード
ord-735061efe95b4db793efb7d3103e2486
出典データセット
uspto-grants-1977_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04010166

反応ノート

読み込み中…

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