8-amino-5H-benzo[b][1,4]benzoxazepin-6-one → HCID 178465553、化合物

HRID 895982ノート

反応式

HRID 895982 の反応式
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]2[O:11][C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=3[NH:8][C:7](=[O:16])[C:6]=2[CH:17]=1.Br.C1C2C(=CC=CC=2)C=CC=1CS[C:31](=[NH:33])[CH3:32]>C(O)C>[O:16]=[C:7]1[C:6]2[CH:17]=[C:2]([NH:1][C:31](=[NH:33])[CH3:32])[CH:3]=[CH:4][C:5]=2[O:11][C:10]2[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=2[NH:8]1

参加物

4

反応物 2

HCID 27563998-amino-5H-benzo[b][1,4]benzoxazepin-6-oneHCID 221387052-Naphthylmethyl ethanimidothioate hydrobromide

生成物 1

HCID 178465553HCID 178465553、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a stirred solution of 2-amino-10H-dibenzo[b,f][1,4]oxazepin-11-one (Example 4, 50 mg, 0.22 mmol) in 4 mL of ethanol at 0° C. was added thioacetimidic acid naphthalen-2-ylmethyl ester hydrobromide (65 mg, 0.22 mmol). The reaction was warmed to room temperature overnight. The mixture was concentrated at reduced pressure and partitioned between water (5 mL) and ethyl acetate (25 mL). The aqueous layer was separated and evaporated under vacuum (yield 70 mg, 92%). H1 NMR (DMSO d6) δ: 11.15 (bs, 1H), 10.68 (s, 1H), 9.44 (bs, 1H), 8.56 (bs, 1H), 7.71-7.70 (m, 1H), 7.54-7.53 (m, 2H), 7.40-7.36 (m, 1H), 7.20-7.17 (m, 3H), 2.31 (s, 3H), MS (ES): MH+ 268.3.

後処理

  1. concentrationThe mixture was concentrated at reduced pressure
  2. custompartitioned between water (5 mL) and ethyl acetate (25 mL)
  3. customThe aqueous layer was separated
  4. customevaporated under vacuum (yield 70 mg, 92%)

出典と根拠

ORDレコード
ord-d1e932c3f07547b5934f1964769a7d45
出典データセット
uspto-grants-2005_07
特許番号
US06919328B1

反応ノート

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