4-[(4-Dipropylaminobutyl)methylamino]methylbenzonitrile → HCID 67316320、化合物

HRID 1012565ノート

反応式

HRID 1012565 の反応式
[CH2:1]([N:4]([CH2:20][CH2:21][CH3:22])[CH2:5][CH2:6][CH2:7][CH2:8][N:9]([CH2:11][C:12]1[CH:19]=[CH:18][C:15]([C:16]#[N:17])=[CH:14][CH:13]=1)[CH3:10])[CH2:2][CH3:3].[ClH:23].CO>CO>[ClH:23].[CH2:20]([N:4]([CH2:1][CH2:2][CH3:3])[CH2:5][CH2:6][CH2:7][CH2:8][N:9]([CH2:11][C:12]1[CH:13]=[CH:14][C:15]([C:16]#[N:17])=[CH:18][CH:19]=1)[CH3:10])[CH2:21][CH3:22]

参加物

4

反応物 2

HCID 161172934-[(4-Dipropylaminobutyl)methylamino]methylbenzonitrileHCID 21893726Hydrochloride methanol

生成物 1

HCID 67316320HCID 67316320、化合物収率 99%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

100 mg (0.33 mmol) of unpurified 4-[(4-dipropylaminobutyl)methylamino]methylbenzonitrile (2b) synthesized in Example 5 was charged in a 25 ml recovery flask, and dissolved in 3 ml of methanol. After 290 mg (0.80 mmol, 2.4 equivalents) of a 10% hydrochloric acid-methanol solution was added dropwise to the solution under cooling with ice, the mixture was stirred for one hour. The reaction solution was then concentrated. After the addition of 5 ml of methanol to the residue, the mixture was reconcentrated. This operation was repeated twice, thereby obtaining 122 mg of 4-[(4-dipropylaminobutyl)methylamino]methylbenzonitrile hydrochloride (2ba) as a colorless oily substance (yield: 99%).

後処理

  1. temperatureunder cooling with ice
  2. concentrationThe reaction solution was then concentrated
  3. additionAfter the addition of 5 ml of methanol to the residue

出典と根拠

ORDレコード
ord-d7a08052f2da4faeb68b8d86c91eaadd
出典データセット
uspto-grants-2011_07
特許番号
US07977512B2

反応ノート

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