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Water → HCID 20355912, 화합물

HRID 371716
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HRID 371716 반응식
Cl[CH:2]([NH:8][C:9](=[O:11])[CH3:10])[C:3]([Cl:7])([Cl:6])[CH2:4][Cl:5].[NH:12]1[CH:16]=[N:15][CH:14]=[N:13]1.C(N(CC)CC)C.O>O1CCCC1>[NH:8]([CH:2]([N:12]1[CH:16]=[N:15][CH:14]=[N:13]1)[C:3]([Cl:7])([Cl:6])[CH2:4][Cl:5])[C:9]([CH3:10])=[O:11]
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참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 92571H-1,2,4-TriazoleHCID 20355929HCID 20355929, 화합물

생성물 1

HCID 20355912HCID 20355912, 화합물수율 66%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

3.6 gm of N-(1,2,2,3-tetrachloro-n-propyl)-acetamide were dissolved in 30 ml of tetrahydrofuran, and, while stirring, the resulting solution was added dropwise to a solution of 1.05 gm of 1,2,4-triazole and 1.8 gm of triethylamine in 20 ml of tetrahydrofuran. Subsequently, the reaction mixture was stirred for 2 hours at room temperature, then water was added, and the tetrahydrofuran was distilled off in vacuo. The oil thus obtained as a residue crystallized after some time and was recrystallized from methanol/water, yielding 2.7 gm of the compound of the formula ##STR5## having a melting point of 135° C.

후처리

  1. stirringSubsequently, the reaction mixture was stirred for 2 hours at room temperature
  2. distillationthe tetrahydrofuran was distilled off in vacuo
  3. customThe oil thus obtained as a residue
  4. customcrystallized after some time
  5. customwas recrystallized from methanol/water

출처 및 근거

ORD 기록
ord-cc7ba7a949c84e358933e619187a4fce
출처 데이터셋
uspto-grants-1978_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04087533

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