Triethylamine → 3-Dimethylaminophenyl isocyanate

HRID 230557

반응식

HRID 230557 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 117895273-Dimethylaminophenyl isocyanate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
20 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bf812353ccc34e29a55bbe348f993373
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07566736B2

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