Benzoylacetonitrile → HCID 85446889, 화합물

HRID 1085158노트

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HRID 1085158 반응식
[C:1]([CH2:9][C:10]#[N:11])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CC(OCC1C2C(=CC=CC=2)C(COC(C)=O)=C2C=1C=CC=C2)=O.[N:36]([O-])=[O:37].[Na+]>O>[OH:37][N:36]=[C:9]([C:1](=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[C:10]#[N:11]

참가 물질

5

실험 절차

A suspension of benzoylacetonitrile (11.7 g, 80.7 mmol) in a mixture of glacial acetic (34 ml) and water (1 ml) was stirred vigorously at 10° C. whilst an aqueous solution of sodium nitrite (6.1 g, 88.4 mmol in 7 ml) was added dropwise over 30 minutes. The mixture was stirred for 1 hour at room temperature and then poured into iced water (600 ml). The yellow solid which precipitated was filtered off, washed with water (100 ml) and dried, giving the title compound, 7.8 g (56%). m.p. 126°-128° C. (literature m.p. 117°-119° C.; Ger. Offen. 2,722,416 (1978).

후처리

  1. additionwas added dropwise over 30 minutes
  2. customThe yellow solid which precipitated
  3. filtrationwas filtered off
  4. washwashed with water (100 ml)
  5. customdried

출처 및 근거

ORD 기록
ord-6072e71bb257424fbc953473da49965e
출처 데이터셋
uspto-grants-1991_04
특허 번호
US05008263

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