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Hydrazine hydrate (1:1) → HCID 14638227, 화합물

HRID 1253193
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HRID 1253193 반응식
O.[NH2:2][NH2:3].Cl[C:5]1[C:10]2[O:11][CH2:12][C:13](=[O:15])[NH:14][C:9]=2[N:8]=[C:7]([CH3:16])[N:6]=1>C(O)CCC>[NH:2]([C:5]1[C:10]2[O:11][CH2:12][C:13](=[O:15])[NH:14][C:9]=2[N:8]=[C:7]([CH3:16])[N:6]=1)[NH2:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 608089HCID 608089, 화합물

생성물 1

HCID 14638227HCID 14638227, 화합물수율 56.3%

시약·촉매·용매 1

HCID 2631-Butanol용매2회

실험 절차

12.8 ml of 98% hydrazine hydrate dissolved in 40 ml of n-butanol are dropped to a solution of 20 g of 4-chloro-2-methyl-6,7-dihydro-8H-pyrimido[5,4-b][1,4]oxazin-7-one in 320 ml of n-butanol at 117° C. within 30 minutes while stirring. The mixture is stirred for an additional 45 minutes at 117° C., then cooled to room temperature. The precipitate is filtered and washed with water to give 11.66 g (56.3%) of the product, m.p.: 262°-264° C.

후처리

  1. stirringThe mixture is stirred for an additional 45 minutes at 117° C.
  2. filtrationThe precipitate is filtered
  3. washwashed with water

출처 및 근거

ORD 기록
ord-b50c7c1671484566b3146f1fe3404044
출처 데이터셋
uspto-grants-1988_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04748175

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