Hydrochloric Acid → N-(2-(1H-Indene-1-yl)ethyl)hydroxylamine

HRID 1534796ノート

反応式

HRID 1534796 の反応式
[CH:1]1([CH2:10][CH:11]=[N:12][OH:13])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH:3]=[CH:2]1.C([BH3-])#N.[Na+].CN(C1C=CC(N=NC2C=CC(S(O)(=O)=O)=CC=2)=CC=1)C.Cl.[NH4+].[OH-]>CO.O>[CH:1]1([CH2:10][CH2:11][NH:12][OH:13])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH:3]=[CH:2]1

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 11037Benzenesulfonic acid, 4-(2-(4-(dimethylamino)phenyl)diazenyl)-HCID 14923Ammonium HydroxideHCID 5003444Sodium cyanoborohydrideHCID 856179012-(1H-indene-1-yl)acetaldoxime

生成物 1

HCID 19908298N-(2-(1H-Indene-1-yl)ethyl)hydroxylamine

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 962Water溶媒

実験手順

2-(1H-indene-1-yl)acetaldoxime (50 mg, 0.29 mmol) was dissolved in methanol (15 ml) and treated with sodium cyanoborohydride (34 mg, 0.54 mmol). Methyl orange indicator (ca 1 mg) was added, and the pH of the mixture adjusted by addition of 1:1 conc. HCl:MeOH to maintain the indicator color slightly to the red side of the turning point. After ca 1 ml of the acid mixture had been added, the indicator remained red. The reaction was made basic with conc. NH4OH, and water was added. The mixture was extracted with ether and the ether layer was dried over sodium sulfate, filtered, and evaporated to dryness in vacuo to provide N-(2-(1H-indene-1-yl)-ethyl)hydroxylamine.

後処理

  1. additionwas added
  2. extractionThe mixture was extracted with ether
  3. dry with materialthe ether layer was dried over sodium sulfate
  4. filtrationfiltered
  5. customevaporated to dryness in vacuo

出典と根拠

ORDレコード
ord-cdeca3a901b44f63bdb2a148663f4a0f
出典データセット
uspto-grants-1992_02
特許番号
US05091387

反応ノート

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