Triethylamine → 3-Dimethylaminophenyl isocyanate

HRID 230557

反応式

HRID 230557 の反応式
Cl.Cl.[CH3:3][N:4]([CH3:12])[C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([NH2:11])[CH:6]=1.C(N(CC)CC)C.Cl[C:21](Cl)([O:23]C(=O)OC(Cl)(Cl)Cl)Cl>ClCCl>[CH3:3][N:4]([CH3:12])[C:5]1[CH:6]=[C:7]([N:11]=[C:21]=[O:23])[CH:8]=[CH:9][CH:10]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 771241,3-Benzenediamine, N1,N1-dimethyl-, hydrochloride (1:2)HCID 94429Triphosgene

生成物 1

HCID 117895273-Dimethylaminophenyl isocyanate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
20 °C

実験手順

1.46 g (7 mmol) of N1,N1-dimethylbenzene-1,3-diamine dihydrochloride, followed by 9.9 cm3 (71.64 mmol) of triethylamine, are added, at a temperature in the region of 5° C., under an argon atmosphere, to 2.82 g (9.5 mmol) of triphosgene in solution in 150 cm3 of dichloromethane. After stirring for 20 hours at a temperature in the region of 20° C., the reaction mixture is concentrated to dryness under reduced pressure (2.7 kPa), to give a residue which is triturated in 50 cm3 of tetrahydrofuran. After filtration, a solution of 3-dimethylaminophenyl isocyanate in approximately 0.14 N tetrahydrofuran is obtained, which solution is used directly in the subsequent step.

後処理

  1. concentrationthe reaction mixture is concentrated to dryness under reduced pressure (2.7 kPa)
  2. customto give a residue which
  3. customis triturated in 50 cm3 of tetrahydrofuran
  4. filtrationAfter filtration

出典と根拠

ORDレコード
ord-bf812353ccc34e29a55bbe348f993373
出典データセット
uspto-grants-2009_07
特許番号
US07566736B2

関連ノート

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