Triethylamine → HCID 66954038、化合物

HRID 2096983ノート

反応式

HRID 2096983 の反応式
[CH:1]1([NH2:4])[CH2:3][CH2:2]1.ClC(Cl)(O[C:9](=[O:15])OC(Cl)(Cl)Cl)Cl.C(N(CC)CC)C.[NH:24]([C:26]1[C:31]([I:32])=[CH:30][CH:29]=[CH:28][N:27]=1)[NH2:25]>ClCCl>[CH:1]1([NH:4][C:9]([NH:25][NH:24][C:26]2[C:31]([I:32])=[CH:30][CH:29]=[CH:28][N:27]=2)=[O:15])[CH2:3][CH2:2]1

参加物

6

反応物 4

HCID 8471TriethylamineHCID 69828CyclopropylamineHCID 94429TriphosgeneHCID 53402765Pyridine, 2-hydrazinyl-3-iodo-

生成物 1

HCID 66954038HCID 66954038、化合物収率 237.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒4 回

実験手順

Cyclopropylamine (0.12 g, 2.2 mmol) in dichloromethane (3 mL) was added to a solution of triphosgene (0.22 g, 0.74 mmol) in dichloromethane (5 mL) at 0° C. under argon. Triethylamine (0.59 mL, 4.2 mmol) in dichloromethane (3 mL) was then added and the resulting mixture was stirred at room temperature for 2 hours and then cooled to 0° C. 2-Hydrazino-3-iodopyridine (preparation 26b, 0.50 g, 2.1 mmol) in dichloromethane (5 mL) was added and the resulting mixture was stirred at room temperature overnight. The solution was cooled to 0° C. and a solid precipitated. The solid was filtered, washed with diethyl ether and dried to yield the title compound (0.56 g, 83%) as a white solid.

後処理

  1. temperaturecooled to 0° C
  2. stirringthe resulting mixture was stirred at room temperature overnight
  3. temperatureThe solution was cooled to 0° C.
  4. customa solid precipitated
  5. filtrationThe solid was filtered
  6. washwashed with diethyl ether
  7. customdried

出典と根拠

ORDレコード
ord-61b52f27eefd4aadaca7ba8084f8aae4
出典データセット
uspto-grants-2013_05
特許番号
US08450341B2

反応ノート

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