Isopropanol → HCID 89906961、化合物

HRID 924000ノート

反応式

HRID 924000 の反応式
[Br:1][C:2]1[C:3](Cl)=[N:4][CH:5]=[C:6]([CH:21]=1)[C:7]([NH:9][C:10]1[CH:15]=[CH:14][C:13]([O:16][C:17]([F:20])([F:19])[F:18])=[CH:12][CH:11]=1)=[O:8].Cl.[NH2:24][CH2:25][CH2:26][OH:27].CC(O)C.CCN(C(C)C)C(C)C>O>[Br:1][C:2]1[C:3]([NH:24][CH2:25][CH2:26][OH:27])=[N:4][CH:5]=[C:6]([CH:21]=1)[C:7]([NH:9][C:10]1[CH:15]=[CH:14][C:13]([O:16][C:17]([F:20])([F:19])[F:18])=[CH:12][CH:11]=1)=[O:8]

参加物

6

反応物 4

HCID 3776IsopropanolHCID 74819Ethanolamine HydrochlorideHCID 81531DiisopropylethylamineHCID 867025955-bromo-6-chloro-N-(4-(trifluoromethoxy)phenyl)nicotinamide

生成物 1

HCID 89906961HCID 89906961、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 5-bromo-6-chloro-N-(4-(trifluoromethoxy)phenyl)nicotinamide (Stage 12.2, 0.5 g, 1.264 mmol), 2-aminoethanol hydrochloride (0.123 g, 1.896 mmol), iPrOH (4 mL) and DIPEA (0.442 mL, 0.327 g, 2.53 mmol) were subjected to MW irradiation at 140° C. for 2 h. The vial was cooled to RT and the RM was poured into water (100 mL) and the resulting precipitate was collected by filtration. The obtained solid was washed with water (50 mL) and dried to afford the title compound without further purification. LC-MS (Condition 6) tR=1.14 min, m/z=419.8 [M+H]+.

後処理

  1. customwere subjected to MW irradiation at 140° C. for 2 h
  2. filtrationthe resulting precipitate was collected by filtration
  3. washThe obtained solid was washed with water (50 mL)
  4. customdried

出典と根拠

ORDレコード
ord-92137534bb504ee7bfa715a73df54a02
出典データセット
uspto-grants-2016_03
特許番号
US09278981B2

反応ノート

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