Benzoylacetonitrile → HCID 85446889、化合物

HRID 1085158ノート

反応式

HRID 1085158 の反応式
[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]

参加物

5

反応物 3

HCID 64799BenzoylacetonitrileHCID 613145Acetic acid 10-acetoxymethyl-anthracen-9-ylmethyl esterHCID 23668193Sodium Nitrite

生成物 1

HCID 85446889HCID 85446889、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-6072e71bb257424fbc953473da49965e
出典データセット
uspto-grants-1991_04
特許番号
US05008263

反応ノート

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