Acetic Anhydride → HCID 18432836, 화합물

HRID 2305377노트

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HRID 2305377 반응식
[C:1]([CH2:3][C:4]([OH:6])=O)#[N:2].C(OC(=O)C)(=O)C.[Cl:14][C:15]1[CH:25]=[CH:24][C:18]([CH2:19][NH:20][C:21]([NH2:23])=[O:22])=[CH:17][CH:16]=1>C1(C)C=CC=CC=1>[Cl:14][C:15]1[CH:25]=[CH:24][C:18]([CH2:19][NH:20][C:21]([NH:23][C:4](=[O:6])[CH2:3][C:1]#[N:2])=[O:22])=[CH:17][CH:16]=1

참가 물질

5

반응물 3

HCID 7918Acetic Anhydride2회HCID 9740Cyanoacetic acidHCID 1484508N-(4-chlorobenzyl)urea

생성물 1

HCID 18432836HCID 18432836, 화합물수율 85.9%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

68.7 g of 98% cyanoacetic acid and 155 ml of acetic anhydride were kept at 65° C. for 30 minutes. 4-chlorobenzylurea (132.9 g) was added in portions over 10 minutes. After 2 hrs. at 70-75° C., further acetic anhydride (25 ml) was added. After a further 15 minutes,90 ml of toluene was added, cooled to room temperature, the solid collected and washed with toluene to give the title compound (155.60 g) as a white-solid mp 203-6° C.

후처리

  1. waitAfter a further 15 minutes
  2. customthe solid collected
  3. washwashed with toluene

출처 및 근거

ORD 기록
ord-fe1e4a46ed4d48839a2ab3b30d18a03b
출처 데이터셋
uspto-grants-2002_08
특허 번호
US06440979B1

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