Phenyl isocyanate → HCID 69748017、化合物

HRID 1062387ノート

反応式

HRID 1062387 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([NH2:8])[CH:5]=[CH:4][C:3]=1[NH:9][C:10](=[O:18])[C@:11]([OH:17])([CH3:16])[C:12]([F:15])([F:14])[F:13].[C:19]1([N:25]=[C:26]=[O:27])[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>C(OCC)C>[Cl:1][C:2]1[CH:7]=[C:6]([NH:8][C:26]([NH:25][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[O:27])[CH:5]=[CH:4][C:3]=1[NH:9][C:10](=[O:18])[C@:11]([OH:17])([CH3:16])[C:12]([F:13])([F:15])[F:14]

参加物

4

反応物 2

HCID 7672Phenyl isocyanateHCID 54520116HCID 54520116、化合物

生成物 1

HCID 69748017HCID 69748017、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

A mixture of (R)-N-[2-chloro-4-aminophenyl]-2-hydroxy-2-methyl-3,3,3-trifluoropropanamide (Example 208) (0.198 g) and phenyl isocyanate (0.09 ml) in diethyl ether (10 ml) was stirred for 22 hours then evaporated to dryness. The residue was partitioned between water (25 ml) and ethyl acetate (50 ml). The organic phase was washed with brine (25 ml), dried and concentrated by evaporation to give the title compound (170 mg) as a foam. NMR: 1.66 (s, 3H), 7.04 (t, 1H), 7.35 (m, 3H), 7.52 (d, 1H), 7.71 (s, 1H), 7.86 (m, 2H), 8.77 (s, 1H), 8.92 (s, 1H), 9.63 (s, 1H); MS (ESP−): 400.

後処理

  1. customthen evaporated to dryness
  2. customThe residue was partitioned between water (25 ml) and ethyl acetate (50 ml)
  3. washThe organic phase was washed with brine (25 ml)
  4. customdried
  5. concentrationconcentrated by evaporation

出典と根拠

ORDレコード
ord-6ac79108a19d4bb5838eccec8c740360
出典データセット
uspto-grants-2005_11
特許番号
US06960688B2

反応ノート

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